Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_section_title ; The effect of mu-CN linkage isomerism and ancillary ligand set on directional metal-metal charge-transfer in cyanide-bridged dimanganese complexes ; loop_ _publ_author_name 'N. Connelly' 'Chris Adams' 'Kirsty Anderson' 'Estefania Llames-Rey' 'A. Orpen' 'Rowena L. Paul' #========================================================================== # 4. TEXT # # # N. G. CONNELLY # data_1+ _database_code_depnum_ccdc_archive 'CCDC 166635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H59 F6 Mn2 N3 O7 P4' _chemical_formula_weight 1137.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.077(4) _cell_length_b 13.608(4) _cell_length_c 19.195(3) _cell_angle_alpha 103.00(3) _cell_angle_beta 100.75(3) _cell_angle_gamma 97.00(2) _cell_volume 2728.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 290 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872551 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23701 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9579 _reflns_number_gt 8055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+3.9587P] 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 9579 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.04134(4) -1.58129(3) -0.79708(3) 0.03482(13) Uani 1 1 d . . . Mn2 Mn -0.28998(4) -1.31725(3) -0.68926(2) 0.02804(12) Uani 1 1 d . . . P1 P -0.37400(7) -1.29535(5) -0.80235(4) 0.02724(16) Uani 1 1 d . . . P2 P -0.43497(7) -1.21403(5) -0.67415(4) 0.02975(17) Uani 1 1 d . . . P3 P -0.22094(8) -1.32267(7) -0.57463(4) 0.0397(2) Uani 1 1 d . . . N1 N -0.1778(2) -1.40986(19) -0.72977(13) 0.0325(5) Uani 1 1 d . . . N2 N 0.0323(3) -1.5956(2) -0.71755(16) 0.0422(6) Uani 1 1 d . . . N3 N -0.2751(3) -1.7363(2) -0.81046(18) 0.0541(8) Uani 1 1 d . A . O1 O 0.0908(3) -1.6059(2) -0.66298(15) 0.0625(7) Uani 1 1 d . . . O2 O -0.1021(2) -1.1291(2) -0.66391(15) 0.0599(7) Uani 1 1 d . . . O3 O -0.4712(2) -1.50935(17) -0.71357(13) 0.0465(6) Uani 1 1 d . . . O4 O -0.1439(3) -1.4114(2) -0.55902(14) 0.0622(7) Uani 1 1 d . . . O5 O -0.3291(2) -1.3310(2) -0.53042(12) 0.0484(6) Uani 1 1 d . . . O6 O -0.1274(2) -1.2256(2) -0.52024(14) 0.0616(7) Uani 1 1 d . . . C1 C -0.1264(3) -1.4721(2) -0.75619(17) 0.0330(6) Uani 1 1 d . . . C2 C 0.2449(4) -1.5986(6) -0.7995(3) 0.100(2) Uani 1 1 d . . . H2A H 0.3082 -1.5898 -0.8282 0.150 Uiso 1 1 calc R . . H2B H 0.2392 -1.6669 -0.7904 0.150 Uiso 1 1 calc R . . H2C H 0.2683 -1.5466 -0.7526 0.150 Uiso 1 1 calc R . . C3 C 0.1210(3) -1.5872(4) -0.8414(2) 0.0559(10) Uani 1 1 d . . . C4 C 0.0776(4) -1.4924(3) -0.8432(2) 0.0546(10) Uani 1 1 d . . . H4A H 0.1262 -1.4222 -0.8187 0.065 Uiso 1 1 calc R . . C5 C -0.0405(4) -1.5156(3) -0.89026(19) 0.0513(9) Uani 1 1 d . . . H5A H -0.0924 -1.4644 -0.9033 0.062 Uiso 1 1 calc R . . C6 C -0.0733(4) -1.6205(3) -0.9161(2) 0.0556(9) Uani 1 1 d . . . H6A H -0.1529 -1.6579 -0.9509 0.067 Uiso 1 1 calc R . . C7 C 0.0238(4) -1.6657(3) -0.8863(2) 0.0575(10) Uani 1 1 d . . . H7A H 0.0264 -1.7407 -0.8975 0.069 Uiso 1 1 calc R . . C8 C -0.1888(3) -1.6775(2) -0.80696(19) 0.0455(8) Uani 1 1 d . . . C9 C -0.3830(4) -1.8137(3) -0.8165(3) 0.0604(11) Uani 1 1 d . . . C10 C -0.4881(6) -1.7974(6) -0.8705(5) 0.083(3) Uani 0.754(13) 1 d P A 1 H10A H -0.5047 -1.7277 -0.8546 0.124 Uiso 0.754(13) 1 calc PR A 1 H10B H -0.5627 -1.8467 -0.8741 0.124 Uiso 0.754(13) 1 calc PR A 1 H10C H -0.4664 -1.8070 -0.9185 0.124 Uiso 0.754(13) 1 calc PR A 1 C11 C -0.4149(9) -1.7887(7) -0.7375(5) 0.099(3) Uani 0.754(13) 1 d P A 1 H11A H -0.3443 -1.7963 -0.7010 0.149 Uiso 0.754(13) 1 calc PR A 1 H11B H -0.4892 -1.8361 -0.7379 0.149 Uiso 0.754(13) 1 calc PR A 1 H11C H -0.4308 -1.7183 -0.7251 0.149 Uiso 0.754(13) 1 calc PR A 1 C12 C -0.3493(10) -1.9160(7) -0.8327(9) 0.118(6) Uani 0.754(13) 1 d P A 1 H12A H -0.2778 -1.9189 -0.7950 0.176 Uiso 0.754(13) 1 calc PR A 1 H12B H -0.3274 -1.9305 -0.8807 0.176 Uiso 0.754(13) 1 calc PR A 1 H12C H -0.4203 -1.9671 -0.8334 0.176 Uiso 0.754(13) 1 calc PR A 1 C10' C -0.485(3) -1.7764(18) -0.803(2) 0.120(17) Uani 0.246(13) 1 d P A 2 H10D H -0.4854 -1.7684 -0.7507 0.180 Uiso 0.246(13) 1 calc PR A 2 H10E H -0.5593 -1.8238 -0.8329 0.180 Uiso 0.246(13) 1 calc PR A 2 H10F H -0.4835 -1.7097 -0.8141 0.180 Uiso 0.246(13) 1 calc PR A 2 C11' C -0.412(2) -1.873(2) -0.9086(13) 0.109(13) Uani 0.246(13) 1 d P A 2 H11D H -0.3351 -1.8916 -0.9215 0.163 Uiso 0.246(13) 1 calc PR A 2 H11E H -0.4426 -1.8256 -0.9370 0.163 Uiso 0.246(13) 1 calc PR A 2 H11F H -0.4754 -1.9344 -0.9199 0.163 Uiso 0.246(13) 1 calc PR A 2 C12' C -0.328(4) -1.894(3) -0.787(3) 0.16(3) Uani 0.246(13) 1 d P A 2 H12D H -0.2863 -1.8650 -0.7351 0.238 Uiso 0.246(13) 1 calc PR A 2 H12E H -0.2664 -1.9177 -0.8145 0.238 Uiso 0.246(13) 1 calc PR A 2 H12F H -0.3935 -1.9512 -0.7912 0.238 Uiso 0.246(13) 1 calc PR A 2 C13 C -0.1738(3) -1.2019(2) -0.67386(17) 0.0379(7) Uani 1 1 d . . . C14 C -0.4037(3) -1.4342(2) -0.70376(16) 0.0323(6) Uani 1 1 d . . . C15 C -0.2796(3) -1.2464(2) -0.85954(15) 0.0319(6) Uani 1 1 d . . . C16 C -0.1559(3) -1.2601(2) -0.85278(18) 0.0391(7) Uani 1 1 d . . . H16A H -0.1209 -1.2955 -0.8187 0.047 Uiso 1 1 calc R . . C17 C -0.0837(3) -1.2223(3) -0.8956(2) 0.0514(9) Uani 1 1 d . . . H17A H 0.0003 -1.2328 -0.8915 0.062 Uiso 1 1 calc R . . C18 C -0.1336(4) -1.1693(3) -0.9444(2) 0.0549(10) Uani 1 1 d . . . H18A H -0.0835 -1.1429 -0.9733 0.066 Uiso 1 1 calc R . . C19 C -0.2557(4) -1.1546(3) -0.95116(19) 0.0503(9) Uani 1 1 d . . . H19A H -0.2896 -1.1180 -0.9847 0.060 Uiso 1 1 calc R . . C20 C -0.3296(3) -1.1932(2) -0.90887(17) 0.0410(7) Uani 1 1 d . . . H20A H -0.4138 -1.1833 -0.9137 0.049 Uiso 1 1 calc R . . C21 C -0.4907(3) -1.3969(2) -0.86678(15) 0.0302(6) Uani 1 1 d . . . C22 C -0.6122(3) -1.3842(3) -0.89306(16) 0.0387(7) Uani 1 1 d . . . H22A H -0.6378 -1.3202 -0.8778 0.046 Uiso 1 1 calc R . . C23 C -0.6959(3) -1.4666(3) -0.94214(18) 0.0493(9) Uani 1 1 d . . . H23A H -0.7792 -1.4586 -0.9600 0.059 Uiso 1 1 calc R . . C24 C -0.6587(4) -1.5594(3) -0.96488(18) 0.0514(9) Uani 1 1 d . . . H24A H -0.7164 -1.6150 -0.9982 0.062 Uiso 1 1 calc R . . C25 C -0.5383(4) -1.5719(3) -0.93950(17) 0.0472(8) Uani 1 1 d . . . H25A H -0.5127 -1.6356 -0.9560 0.057 Uiso 1 1 calc R . . C26 C -0.4547(3) -1.4916(2) -0.89000(16) 0.0381(7) Uani 1 1 d . . . H26A H -0.3723 -1.5009 -0.8717 0.046 Uiso 1 1 calc R . . C27 C -0.4526(3) -1.1902(2) -0.76614(16) 0.0352(7) Uani 1 1 d . . . H27A H -0.5409 -1.1996 -0.7921 0.042 Uiso 1 1 calc R . . H27B H -0.4079 -1.1222 -0.7653 0.042 Uiso 1 1 calc R . . C28 C -0.4057(3) -1.0856(2) -0.61176(17) 0.0377(7) Uani 1 1 d . . . C29 C -0.3384(4) -1.0681(3) -0.54077(19) 0.0546(9) Uani 1 1 d . . . H29A H -0.3044 -1.1220 -0.5246 0.065 Uiso 1 1 calc R . . C30 C -0.3203(4) -0.9708(3) -0.4925(2) 0.0700(12) Uani 1 1 d . . . H30A H -0.2745 -0.9594 -0.4435 0.084 Uiso 1 1 calc R . . C31 C -0.3670(5) -0.8933(3) -0.5147(3) 0.0708(13) Uani 1 1 d . . . H31A H -0.3529 -0.8274 -0.4818 0.085 Uiso 1 1 calc R . . C32 C -0.4352(5) -0.9098(3) -0.5853(3) 0.0728(13) Uani 1 1 d . . . H32A H -0.4693 -0.8554 -0.6007 0.087 Uiso 1 1 calc R . . C33 C -0.4545(4) -1.0060(3) -0.6343(2) 0.0559(10) Uani 1 1 d . . . H33G H -0.5011 -1.0169 -0.6830 0.067 Uiso 1 1 calc R . . C34 C -0.5929(3) -1.2638(2) -0.66729(16) 0.0343(6) Uani 1 1 d . . . C35 C -0.6962(3) -1.2260(3) -0.6978(2) 0.0458(8) Uani 1 1 d . . . H35A H -0.6864 -1.1767 -0.7253 0.055 Uiso 1 1 calc R . . C36 C -0.8139(3) -1.2610(3) -0.6879(2) 0.0542(10) Uani 1 1 d . . . H36A H -0.8841 -1.2346 -0.7082 0.065 Uiso 1 1 calc R . . C37 C -0.8293(3) -1.3334(3) -0.6489(2) 0.0553(10) Uani 1 1 d . . . H37F H -0.9099 -1.3573 -0.6427 0.066 Uiso 1 1 calc R . . C38 C -0.7273(3) -1.3713(3) -0.6187(2) 0.0498(9) Uani 1 1 d . . . H38A H -0.7379 -1.4214 -0.5920 0.060 Uiso 1 1 calc R . . C39 C -0.6092(3) -1.3361(2) -0.62743(17) 0.0388(7) Uani 1 1 d . . . H39A H -0.5392 -1.3617 -0.6060 0.047 Uiso 1 1 calc R . . C40 C 0.0003(5) -1.2073(6) -0.4974(4) 0.131(3) Uani 1 1 d . . . H40A H 0.0367 -1.1830 -0.5351 0.158 Uiso 1 1 calc R . . H40B H 0.0285 -1.2727 -0.4941 0.158 Uiso 1 1 calc R . . C41 C 0.0473(5) -1.1354(6) -0.4297(3) 0.130(3) Uani 1 1 d . . . H41A H 0.1378 -1.1314 -0.4156 0.195 Uiso 1 1 calc R . . H41B H 0.0084 -1.1565 -0.3923 0.195 Uiso 1 1 calc R . . H41C H 0.0285 -1.0681 -0.4338 0.195 Uiso 1 1 calc R . . C42 C -0.3026(4) -1.3211(5) -0.4515(2) 0.0774(14) Uani 1 1 d . . . H42A H -0.2722 -1.2484 -0.4250 0.093 Uiso 1 1 calc R . . H42B H -0.2365 -1.3608 -0.4384 0.093 Uiso 1 1 calc R . . C43 C -0.4155(5) -1.3589(4) -0.4297(2) 0.0713(12) Uani 1 1 d . . . H43A H -0.3989 -1.3462 -0.3762 0.107 Uiso 1 1 calc R . . H43B H -0.4405 -1.4325 -0.4520 0.107 Uiso 1 1 calc R . . H43C H -0.4827 -1.3232 -0.4462 0.107 Uiso 1 1 calc R . . C44 C -0.1985(7) -1.5182(4) -0.5911(3) 0.106(2) Uani 1 1 d . . . H44A H -0.2903 -1.5241 -0.5987 0.127 Uiso 1 1 calc R . . H44B H -0.1791 -1.5386 -0.6401 0.127 Uiso 1 1 calc R . . C45 C -0.1633(8) -1.5856(5) -0.5538(4) 0.147(4) Uani 1 1 d . . . H45A H -0.2135 -1.6533 -0.5780 0.221 Uiso 1 1 calc R . . H45B H -0.1756 -1.5640 -0.5037 0.221 Uiso 1 1 calc R . . H45C H -0.0750 -1.5889 -0.5522 0.221 Uiso 1 1 calc R . . O999 O -0.7832(7) -0.8247(4) -0.7212(3) 0.171(3) Uani 1 1 d . . . C997 C -0.8567(7) -0.9014(4) -0.7382(3) 0.0963(17) Uani 1 1 d . . . C998 C -0.8335(7) -0.9930(6) -0.7174(5) 0.136(3) Uani 1 1 d . . . H99A H -0.7503 -0.9806 -0.6853 0.204 Uiso 1 1 calc R . . H99B H -0.8378 -1.0476 -0.7614 0.204 Uiso 1 1 calc R . . H99C H -0.8963 -1.0137 -0.6913 0.204 Uiso 1 1 calc R . . C999 C -0.9849(8) -0.9072(7) -0.7865(5) 0.163(4) Uani 1 1 d . . . H99D H -1.0177 -0.8444 -0.7698 0.244 Uiso 1 1 calc R . . H99E H -1.0419 -0.9663 -0.7835 0.244 Uiso 1 1 calc R . . H99F H -0.9775 -0.9146 -0.8375 0.244 Uiso 1 1 calc R . . P5 P -0.72994(11) -1.10288(9) -0.92451(11) 0.0998(6) Uani 1 1 d . . . F1 F -0.8240(5) -1.0350(3) -0.8929(3) 0.184(3) Uani 1 1 d . . . F2 F -0.6420(4) -1.1773(4) -0.9535(4) 0.199(3) Uani 1 1 d . . . F3 F -0.7804(3) -1.1872(3) -0.8847(3) 0.162(2) Uani 1 1 d . . . F4 F -0.6739(5) -1.0190(3) -0.9561(3) 0.199(3) Uani 1 1 d . . . F5 F -0.6332(4) -1.0591(4) -0.8497(3) 0.202(3) Uani 1 1 d . . . F6 F -0.8288(4) -1.1488(3) -0.9933(3) 0.205(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0297(2) 0.0319(2) 0.0387(3) 0.00284(19) 0.00473(19) 0.00552(18) Mn2 0.0271(2) 0.0286(2) 0.0253(2) 0.00338(17) 0.00345(17) 0.00321(17) P1 0.0290(4) 0.0270(4) 0.0242(4) 0.0029(3) 0.0059(3) 0.0055(3) P2 0.0324(4) 0.0278(4) 0.0260(4) 0.0004(3) 0.0072(3) 0.0046(3) P3 0.0380(4) 0.0466(5) 0.0290(4) 0.0075(3) -0.0013(3) 0.0047(4) N1 0.0276(12) 0.0344(13) 0.0330(13) 0.0074(11) 0.0029(10) 0.0044(11) N2 0.0381(15) 0.0392(15) 0.0509(17) 0.0111(13) 0.0110(13) 0.0113(12) N3 0.0475(18) 0.0391(16) 0.066(2) 0.0070(14) 0.0061(15) -0.0057(14) O1 0.0631(17) 0.0753(19) 0.0540(16) 0.0292(14) 0.0036(14) 0.0210(14) O2 0.0571(16) 0.0496(15) 0.0586(16) 0.0031(12) 0.0093(13) -0.0200(13) O3 0.0457(13) 0.0365(12) 0.0526(14) 0.0079(10) 0.0102(11) -0.0034(11) O4 0.0703(18) 0.0729(18) 0.0446(14) 0.0208(13) -0.0018(13) 0.0287(15) O5 0.0482(14) 0.0666(16) 0.0270(11) 0.0136(11) 0.0028(10) 0.0024(12) O6 0.0479(15) 0.0690(17) 0.0489(15) 0.0043(13) -0.0135(12) -0.0054(13) C1 0.0262(14) 0.0324(15) 0.0362(16) 0.0068(13) 0.0014(12) 0.0009(12) C2 0.044(2) 0.203(7) 0.071(3) 0.051(4) 0.026(2) 0.045(3) C3 0.0350(18) 0.093(3) 0.043(2) 0.016(2) 0.0153(15) 0.0160(19) C4 0.061(2) 0.055(2) 0.041(2) 0.0027(17) 0.0210(18) -0.0093(18) C5 0.058(2) 0.059(2) 0.0423(19) 0.0141(17) 0.0141(17) 0.0199(18) C6 0.052(2) 0.067(2) 0.0386(19) 0.0029(17) 0.0014(16) 0.0076(19) C7 0.071(3) 0.052(2) 0.049(2) 0.0003(17) 0.0192(19) 0.0212(19) C8 0.0433(19) 0.0355(17) 0.051(2) 0.0017(15) 0.0062(16) 0.0060(15) C9 0.040(2) 0.043(2) 0.089(3) 0.021(2) -0.0022(19) -0.0079(16) C10 0.051(4) 0.076(5) 0.113(7) 0.040(5) -0.010(4) -0.008(3) C11 0.093(6) 0.104(6) 0.096(6) 0.037(5) 0.022(5) -0.030(5) C12 0.054(5) 0.037(4) 0.241(17) 0.023(6) 0.000(7) 0.001(3) C10' 0.10(2) 0.061(13) 0.21(5) 0.02(2) 0.08(3) 0.013(13) C11' 0.091(18) 0.11(2) 0.083(16) -0.016(13) 0.016(13) -0.064(17) C12' 0.09(2) 0.11(3) 0.26(6) 0.12(4) -0.04(3) -0.06(2) C13 0.0376(17) 0.0409(17) 0.0312(16) 0.0031(13) 0.0065(13) 0.0050(14) C14 0.0319(15) 0.0360(16) 0.0285(15) 0.0055(12) 0.0070(12) 0.0089(13) C15 0.0368(16) 0.0274(14) 0.0275(14) 0.0013(11) 0.0082(12) -0.0015(12) C16 0.0364(17) 0.0397(17) 0.0382(17) 0.0074(14) 0.0080(13) 0.0000(13) C17 0.0412(19) 0.058(2) 0.051(2) 0.0089(17) 0.0155(16) -0.0069(16) C18 0.065(3) 0.049(2) 0.045(2) 0.0087(17) 0.0193(18) -0.0157(18) C19 0.069(3) 0.0422(19) 0.0385(18) 0.0142(15) 0.0117(17) -0.0003(17) C20 0.0467(19) 0.0375(17) 0.0364(17) 0.0073(14) 0.0078(14) 0.0042(14) C21 0.0344(15) 0.0325(15) 0.0216(13) 0.0047(11) 0.0071(11) 0.0003(12) C22 0.0345(16) 0.0500(19) 0.0302(16) 0.0091(14) 0.0058(13) 0.0056(14) C23 0.0371(18) 0.070(2) 0.0333(17) 0.0127(17) 0.0008(14) -0.0061(17) C24 0.057(2) 0.053(2) 0.0305(17) 0.0029(15) 0.0044(16) -0.0199(18) C25 0.070(2) 0.0350(17) 0.0311(17) 0.0022(14) 0.0128(16) -0.0034(16) C26 0.0447(18) 0.0349(16) 0.0317(16) 0.0048(13) 0.0076(14) 0.0036(13) C27 0.0423(17) 0.0336(15) 0.0312(15) 0.0060(12) 0.0095(13) 0.0144(13) C28 0.0389(17) 0.0322(15) 0.0377(17) -0.0034(13) 0.0172(14) 0.0002(13) C29 0.065(2) 0.048(2) 0.0395(19) -0.0079(16) 0.0116(17) 0.0034(18) C30 0.078(3) 0.065(3) 0.048(2) -0.018(2) 0.016(2) -0.005(2) C31 0.087(3) 0.042(2) 0.072(3) -0.019(2) 0.041(3) -0.007(2) C32 0.104(4) 0.0335(19) 0.083(3) 0.001(2) 0.042(3) 0.014(2) C33 0.076(3) 0.0359(18) 0.055(2) 0.0009(16) 0.023(2) 0.0136(18) C34 0.0314(15) 0.0314(15) 0.0318(15) -0.0063(12) 0.0059(12) 0.0026(12) C35 0.0375(18) 0.0431(18) 0.050(2) 0.0006(15) 0.0057(15) 0.0078(14) C36 0.0331(18) 0.054(2) 0.061(2) -0.0088(18) 0.0022(16) 0.0082(16) C37 0.0350(19) 0.052(2) 0.062(2) -0.0156(18) 0.0155(17) -0.0069(16) C38 0.047(2) 0.0453(19) 0.050(2) -0.0032(16) 0.0193(17) -0.0044(16) C39 0.0382(17) 0.0371(16) 0.0361(17) -0.0008(13) 0.0098(13) 0.0030(13) C40 0.042(3) 0.145(6) 0.143(6) -0.063(5) -0.005(3) -0.003(3) C41 0.062(3) 0.172(7) 0.095(4) -0.044(4) -0.007(3) -0.031(4) C42 0.069(3) 0.129(4) 0.031(2) 0.026(2) 0.0057(19) 0.004(3) C43 0.089(3) 0.088(3) 0.042(2) 0.020(2) 0.025(2) 0.009(3) C44 0.194(7) 0.064(3) 0.055(3) 0.016(2) -0.006(3) 0.057(4) C45 0.200(8) 0.115(5) 0.094(4) 0.066(4) -0.036(5) -0.065(5) O999 0.229(7) 0.095(3) 0.145(5) -0.013(3) 0.025(4) -0.037(4) C997 0.122(5) 0.066(3) 0.084(4) -0.001(3) 0.017(3) 0.003(3) C998 0.134(6) 0.139(6) 0.181(8) 0.093(6) 0.055(6) 0.069(5) C999 0.160(8) 0.152(7) 0.172(8) 0.036(6) -0.010(6) 0.092(6) P5 0.0428(6) 0.0512(7) 0.1897(17) 0.0484(9) -0.0279(8) -0.0016(5) F1 0.221(5) 0.116(3) 0.173(4) -0.011(3) -0.049(4) 0.110(4) F2 0.125(3) 0.227(5) 0.386(9) 0.236(6) 0.157(5) 0.121(4) F3 0.083(2) 0.102(3) 0.348(7) 0.099(4) 0.106(3) 0.0278(19) F4 0.235(5) 0.112(3) 0.203(5) 0.117(3) -0.102(4) -0.066(3) F5 0.110(3) 0.223(5) 0.258(6) 0.176(5) -0.088(4) -0.045(3) F6 0.096(3) 0.121(3) 0.281(7) -0.097(4) -0.069(3) 0.020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N2 1.656(3) . ? Mn1 C8 1.916(4) . ? Mn1 C1 1.951(3) . ? Mn1 C4 2.124(4) . ? Mn1 C3 2.131(4) . ? Mn1 C7 2.133(4) . ? Mn1 C5 2.173(4) . ? Mn1 C6 2.176(4) . ? Mn2 C13 1.834(3) . ? Mn2 C14 1.839(3) . ? Mn2 N1 2.010(3) . ? Mn2 P3 2.2114(10) . ? Mn2 P2 2.2753(11) . ? Mn2 P1 2.2960(10) . ? P1 C21 1.819(3) . ? P1 C15 1.825(3) . ? P1 C27 1.836(3) . ? P2 C28 1.835(3) . ? P2 C34 1.837(3) . ? P2 C27 1.846(3) . ? P3 O6 1.597(3) . ? P3 O5 1.600(3) . ? P3 O4 1.610(3) . ? N1 C1 1.153(4) . ? N2 O1 1.171(4) . ? N3 C8 1.150(4) . ? N3 C9 1.463(5) . ? O2 C13 1.147(4) . ? O3 C14 1.146(4) . ? O4 C44 1.450(6) . ? O5 C42 1.459(4) . ? O6 C40 1.375(5) . ? C2 C3 1.500(6) . ? C3 C7 1.415(6) . ? C3 C4 1.436(6) . ? C4 C5 1.399(5) . ? C5 C6 1.380(5) . ? C6 C7 1.397(6) . ? C9 C10' 1.34(2) . ? C9 C12 1.466(10) . ? C9 C12' 1.48(4) . ? C9 C10 1.482(7) . ? C9 C11 1.592(9) . ? C9 C11' 1.72(2) . ? C15 C20 1.391(4) . ? C15 C16 1.392(4) . ? C16 C17 1.384(5) . ? C17 C18 1.381(5) . ? C18 C19 1.378(6) . ? C19 C20 1.393(5) . ? C21 C22 1.393(4) . ? C21 C26 1.396(4) . ? C22 C23 1.396(5) . ? C23 C24 1.379(6) . ? C24 C25 1.376(5) . ? C25 C26 1.383(5) . ? C28 C29 1.378(5) . ? C28 C33 1.385(5) . ? C29 C30 1.403(5) . ? C30 C31 1.348(7) . ? C31 C32 1.377(7) . ? C32 C33 1.396(5) . ? C34 C39 1.391(4) . ? C34 C35 1.395(5) . ? C35 C36 1.395(5) . ? C36 C37 1.379(6) . ? C37 C38 1.382(6) . ? C38 C39 1.390(5) . ? C40 C41 1.403(7) . ? C42 C43 1.463(6) . ? C44 C45 1.337(7) . ? O999 C997 1.183(7) . ? C997 C998 1.429(8) . ? C997 C999 1.528(9) . ? P5 F6 1.501(4) . ? P5 F4 1.528(4) . ? P5 F5 1.565(5) . ? P5 F2 1.574(5) . ? P5 F1 1.589(5) . ? P5 F3 1.616(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn1 C8 96.14(15) . . ? N2 Mn1 C1 96.34(13) . . ? C8 Mn1 C1 88.62(13) . . ? N2 Mn1 C4 111.63(15) . . ? C8 Mn1 C4 150.73(15) . . ? C1 Mn1 C4 96.98(15) . . ? N2 Mn1 C3 92.58(14) . . ? C8 Mn1 C3 134.28(16) . . ? C1 Mn1 C3 134.84(15) . . ? C4 Mn1 C3 39.44(16) . . ? N2 Mn1 C7 111.56(15) . . ? C8 Mn1 C7 97.22(16) . . ? C1 Mn1 C7 150.56(14) . . ? C4 Mn1 C7 64.74(16) . . ? C3 Mn1 C7 38.76(16) . . ? N2 Mn1 C5 149.54(15) . . ? C8 Mn1 C5 114.12(15) . . ? C1 Mn1 C5 88.08(13) . . ? C4 Mn1 C5 37.97(15) . . ? C3 Mn1 C5 64.25(15) . . ? C7 Mn1 C5 63.16(15) . . ? N2 Mn1 C6 149.28(14) . . ? C8 Mn1 C6 88.03(16) . . ? C1 Mn1 C6 114.22(14) . . ? C4 Mn1 C6 63.44(15) . . ? C3 Mn1 C6 64.03(15) . . ? C7 Mn1 C6 37.81(15) . . ? C5 Mn1 C6 37.00(15) . . ? C13 Mn2 C14 178.72(14) . . ? C13 Mn2 N1 92.66(12) . . ? C14 Mn2 N1 86.45(12) . . ? C13 Mn2 P3 89.41(11) . . ? C14 Mn2 P3 89.73(10) . . ? N1 Mn2 P3 94.22(8) . . ? C13 Mn2 P2 88.18(11) . . ? C14 Mn2 P2 92.91(10) . . ? N1 Mn2 P2 165.33(7) . . ? P3 Mn2 P2 100.43(4) . . ? C13 Mn2 P1 88.94(10) . . ? C14 Mn2 P1 92.03(10) . . ? N1 Mn2 P1 92.83(8) . . ? P3 Mn2 P1 172.82(4) . . ? P2 Mn2 P1 72.53(4) . . ? C21 P1 C15 104.18(13) . . ? C21 P1 C27 108.39(15) . . ? C15 P1 C27 105.51(14) . . ? C21 P1 Mn2 119.15(10) . . ? C15 P1 Mn2 122.94(10) . . ? C27 P1 Mn2 94.66(10) . . ? C28 P2 C34 101.62(14) . . ? C28 P2 C27 104.09(14) . . ? C34 P2 C27 105.53(15) . . ? C28 P2 Mn2 125.36(11) . . ? C34 P2 Mn2 121.79(10) . . ? C27 P2 Mn2 95.09(10) . . ? O6 P3 O5 100.25(15) . . ? O6 P3 O4 99.20(15) . . ? O5 P3 O4 104.06(15) . . ? O6 P3 Mn2 118.18(11) . . ? O5 P3 Mn2 113.32(9) . . ? O4 P3 Mn2 119.07(11) . . ? C1 N1 Mn2 171.6(2) . . ? O1 N2 Mn1 175.9(3) . . ? C8 N3 C9 178.0(4) . . ? C44 O4 P3 120.3(3) . . ? C42 O5 P3 122.3(2) . . ? C40 O6 P3 131.2(3) . . ? N1 C1 Mn1 176.9(3) . . ? C7 C3 C4 106.2(3) . . ? C7 C3 C2 127.8(5) . . ? C4 C3 C2 126.0(4) . . ? C7 C3 Mn1 70.7(2) . . ? C4 C3 Mn1 70.0(2) . . ? C2 C3 Mn1 123.8(3) . . ? C5 C4 C3 107.7(3) . . ? C5 C4 Mn1 72.9(2) . . ? C3 C4 Mn1 70.5(2) . . ? C6 C5 C4 108.9(3) . . ? C6 C5 Mn1 71.6(2) . . ? C4 C5 Mn1 69.1(2) . . ? C5 C6 C7 108.6(3) . . ? C5 C6 Mn1 71.4(2) . . ? C7 C6 Mn1 69.4(2) . . ? C6 C7 C3 108.6(4) . . ? C6 C7 Mn1 72.7(2) . . ? C3 C7 Mn1 70.5(2) . . ? N3 C8 Mn1 177.3(3) . . ? C10' C9 N3 114.8(11) . . ? C10' C9 C12 135.1(12) . . ? N3 C9 C12 109.9(5) . . ? C10' C9 C12' 127(3) . . ? N3 C9 C12' 103.7(13) . . ? C12 C9 C12' 33(2) . . ? C10' C9 C10 52.9(18) . . ? N3 C9 C10 107.8(4) . . ? C12 C9 C10 115.4(7) . . ? C12' C9 C10 143.1(15) . . ? C10' C9 C11 56.2(19) . . ? N3 C9 C11 104.7(4) . . ? C12 C9 C11 109.6(8) . . ? C12' C9 C11 80(2) . . ? C10 C9 C11 108.9(7) . . ? C10' C9 C11' 108(2) . . ? N3 C9 C11' 100.0(7) . . ? C12 C9 C11' 66.0(12) . . ? C12' C9 C11' 99(2) . . ? C10 C9 C11' 57.2(12) . . ? C11 C9 C11' 154.7(8) . . ? O2 C13 Mn2 179.1(3) . . ? O3 C14 Mn2 177.3(3) . . ? C20 C15 C16 119.5(3) . . ? C20 C15 P1 120.5(2) . . ? C16 C15 P1 120.0(2) . . ? C17 C16 C15 120.1(3) . . ? C18 C17 C16 120.1(4) . . ? C19 C18 C17 120.3(3) . . ? C18 C19 C20 120.1(3) . . ? C15 C20 C19 119.9(3) . . ? C22 C21 C26 119.5(3) . . ? C22 C21 P1 123.1(2) . . ? C26 C21 P1 117.4(2) . . ? C21 C22 C23 119.3(3) . . ? C24 C23 C22 120.5(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C21 120.5(3) . . ? P1 C27 P2 94.53(14) . . ? C29 C28 C33 119.1(3) . . ? C29 C28 P2 120.2(3) . . ? C33 C28 P2 120.7(3) . . ? C28 C29 C30 120.0(4) . . ? C31 C30 C29 120.8(4) . . ? C30 C31 C32 119.9(4) . . ? C31 C32 C33 120.2(4) . . ? C28 C33 C32 120.0(4) . . ? C39 C34 C35 119.3(3) . . ? C39 C34 P2 119.5(2) . . ? C35 C34 P2 121.1(3) . . ? C34 C35 C36 119.7(4) . . ? C37 C36 C35 120.6(3) . . ? C36 C37 C38 119.9(3) . . ? C37 C38 C39 120.1(4) . . ? C38 C39 C34 120.4(3) . . ? O6 C40 C41 114.8(5) . . ? O5 C42 C43 110.0(3) . . ? C45 C44 O4 117.3(5) . . ? O999 C997 C998 124.2(8) . . ? O999 C997 C999 119.9(7) . . ? C998 C997 C999 115.9(6) . . ? F6 P5 F4 92.8(3) . . ? F6 P5 F5 175.7(4) . . ? F4 P5 F5 91.2(2) . . ? F6 P5 F2 90.3(3) . . ? F4 P5 F2 92.2(3) . . ? F5 P5 F2 91.1(3) . . ? F6 P5 F1 89.2(2) . . ? F4 P5 F1 92.4(3) . . ? F5 P5 F1 89.1(3) . . ? F2 P5 F1 175.3(3) . . ? F6 P5 F3 92.1(3) . . ? F4 P5 F3 175.1(3) . . ? F5 P5 F3 83.9(3) . . ? F2 P5 F3 87.9(2) . . ? F1 P5 F3 87.5(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.760 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.065 #===END data_2+ _database_code_depnum_ccdc_archive 'CCDC 166636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H59 F6 Mn2 N3 O7 P4' _chemical_formula_weight 1137.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0916(15) _cell_length_b 13.638(2) _cell_length_c 19.076(4) _cell_angle_alpha 102.981(2) _cell_angle_beta 100.441(2) _cell_angle_gamma 97.5250(11) _cell_volume 2720.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 155 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765755 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 28916 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.52 _reflns_number_total 12399 _reflns_number_gt 7612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^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 12399 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.95675(4) -0.07694(3) 0.20358(3) 0.03379(13) Uani 1 1 d . . . Mn2 Mn 0.70957(4) 0.18287(3) 0.31097(2) 0.02827(11) Uani 1 1 d . . . P1 P 0.62705(7) 0.20548(5) 0.19830(4) 0.02783(17) Uani 1 1 d . . . P2 P 0.56481(7) 0.28660(5) 0.32637(4) 0.02973(17) Uani 1 1 d . . . P3 P 0.77757(8) 0.17642(6) 0.42557(4) 0.0392(2) Uani 1 1 d . . . O1 O 1.0905(2) -0.1076(2) 0.33559(14) 0.0609(7) Uani 1 1 d . . . O2 O 0.9059(2) 0.36557(18) 0.33541(14) 0.0583(7) Uani 1 1 d . . . O3 O 0.5300(2) -0.01043(16) 0.28513(12) 0.0450(5) Uani 1 1 d . . . O4 O 0.8527(2) 0.0880(2) 0.44142(13) 0.0612(7) Uani 1 1 d . . . O5 O 0.6703(2) 0.16965(18) 0.47058(12) 0.0485(6) Uani 1 1 d . . . O6 O 0.8736(2) 0.27319(19) 0.47931(14) 0.0639(7) Uani 1 1 d . . . N1 N 0.8716(2) 0.03370(18) 0.24376(14) 0.0339(6) Uani 1 1 d . . . N2 N 1.0307(2) -0.09306(19) 0.28256(15) 0.0403(6) Uani 1 1 d . . . N3 N 0.7224(3) -0.2336(2) 0.19003(17) 0.0517(8) Uani 1 1 d . . . C1 C 0.8164(3) 0.0921(2) 0.27030(15) 0.0305(6) Uani 1 1 d . . . C2 C 1.2413(4) -0.1018(4) 0.2010(2) 0.0819(14) Uani 1 1 d . . . H2A H 1.3030 -0.0966 0.1720 0.123 Uiso 1 1 calc R . . H2B H 1.2320 -0.1681 0.2108 0.123 Uiso 1 1 calc R . . H2C H 1.2672 -0.0500 0.2467 0.123 Uiso 1 1 calc R . . C3 C 1.0187(3) -0.1645(3) 0.11487(19) 0.0506(9) Uani 1 1 d . . . H3A H 1.0173 -0.2384 0.1040 0.061 Uiso 1 1 calc R . . C4 C 0.9251(3) -0.1157(3) 0.08420(19) 0.0534(9) Uani 1 1 d . . . H4A H 0.8462 -0.1503 0.0499 0.064 Uiso 1 1 calc R . . C5 C 0.9637(3) -0.0123(3) 0.10954(19) 0.0500(9) Uani 1 1 d . . . H5A H 0.9165 0.0395 0.0968 0.060 Uiso 1 1 calc R . . C6 C 1.0825(3) 0.0081(3) 0.15755(19) 0.0517(9) Uani 1 1 d . . . H6A H 1.1331 0.0758 0.1818 0.062 Uiso 1 1 calc R . . C7 C 1.1196(3) -0.0875(3) 0.15961(19) 0.0495(9) Uani 1 1 d . . . C8 C 0.8092(3) -0.1747(2) 0.19369(18) 0.0441(8) Uani 1 1 d . . . C9 C 0.6149(3) -0.3119(3) 0.1852(2) 0.0570(10) Uani 1 1 d . . . C10 C 0.5812(6) -0.2880(5) 0.2615(3) 0.126(2) Uani 1 1 d . . . H10A H 0.6465 -0.2998 0.2975 0.190 Uiso 1 1 calc R . . H10B H 0.5045 -0.3315 0.2595 0.190 Uiso 1 1 calc R . . H10C H 0.5715 -0.2177 0.2751 0.190 Uiso 1 1 calc R . . C11 C 0.5112(4) -0.2991(4) 0.1310(4) 0.126(3) Uani 1 1 d . . . H11A H 0.5285 -0.3175 0.0827 0.190 Uiso 1 1 calc R . . H11B H 0.5003 -0.2290 0.1423 0.190 Uiso 1 1 calc R . . H11C H 0.4364 -0.3423 0.1324 0.190 Uiso 1 1 calc R . . C12 C 0.6539(5) -0.4118(3) 0.1730(5) 0.142(3) Uani 1 1 d . . . H12A H 0.6727 -0.4294 0.1250 0.213 Uiso 1 1 calc R . . H12B H 0.5879 -0.4626 0.1760 0.213 Uiso 1 1 calc R . . H12C H 0.7268 -0.4088 0.2098 0.213 Uiso 1 1 calc R . . C13 C 0.8300(3) 0.2952(2) 0.32612(16) 0.0374(7) Uani 1 1 d . . . C14 C 0.5966(3) 0.0657(2) 0.29586(15) 0.0314(6) Uani 1 1 d . . . C15 C 0.7220(3) 0.2548(2) 0.14079(15) 0.0320(6) Uani 1 1 d . . . C16 C 0.8446(3) 0.2392(2) 0.14592(17) 0.0390(7) Uani 1 1 d . . . H16A H 0.8781 0.2033 0.1785 0.047 Uiso 1 1 calc R . . C17 C 0.9164(3) 0.2773(3) 0.1024(2) 0.0507(9) Uani 1 1 d . . . H17A H 0.9981 0.2667 0.1057 0.061 Uiso 1 1 calc R . . C18 C 0.8672(4) 0.3310(3) 0.05438(19) 0.0545(10) Uani 1 1 d . . . H18A H 0.9159 0.3565 0.0254 0.065 Uiso 1 1 calc R . . C19 C 0.7461(4) 0.3471(3) 0.04911(19) 0.0521(9) Uani 1 1 d . . . H19A H 0.7135 0.3838 0.0169 0.063 Uiso 1 1 calc R . . C20 C 0.6728(3) 0.3086(2) 0.09191(17) 0.0401(7) Uani 1 1 d . . . H20A H 0.5908 0.3188 0.0879 0.048 Uiso 1 1 calc R . . C21 C 0.5110(3) 0.1032(2) 0.13350(15) 0.0300(6) Uani 1 1 d . . . C22 C 0.5481(3) 0.0089(2) 0.11062(16) 0.0377(7) Uani 1 1 d . . . H22A H 0.6289 0.0007 0.1286 0.045 Uiso 1 1 calc R . . C23 C 0.4639(3) -0.0724(2) 0.06110(17) 0.0470(9) Uani 1 1 d . . . H23A H 0.4887 -0.1347 0.0452 0.056 Uiso 1 1 calc R . . C24 C 0.3439(3) -0.0607(3) 0.03559(17) 0.0511(9) Uani 1 1 d . . . H24A H 0.2878 -0.1155 0.0028 0.061 Uiso 1 1 calc R . . C25 C 0.3058(3) 0.0309(3) 0.05787(17) 0.0499(9) Uani 1 1 d . . . H25A H 0.2244 0.0378 0.0402 0.060 Uiso 1 1 calc R . . C26 C 0.3898(3) 0.1143(2) 0.10738(16) 0.0399(7) Uani 1 1 d . . . H26A H 0.3643 0.1765 0.1225 0.048 Uiso 1 1 calc R . . C27 C 0.5485(3) 0.3099(2) 0.23422(16) 0.0362(7) Uani 1 1 d . . . H27A H 0.4623 0.3002 0.2085 0.043 Uiso 1 1 calc R . . H27B H 0.5926 0.3766 0.2350 0.043 Uiso 1 1 calc R . . C28 C 0.5951(3) 0.4146(2) 0.38919(17) 0.0372(7) Uani 1 1 d . . . C29 C 0.6638(4) 0.4324(3) 0.45970(19) 0.0553(10) Uani 1 1 d . . . H29A H 0.6971 0.3797 0.4752 0.066 Uiso 1 1 calc R . . C30 C 0.6839(4) 0.5295(3) 0.5084(2) 0.0682(12) Uani 1 1 d . . . H30A H 0.7310 0.5411 0.5560 0.082 Uiso 1 1 calc R . . C31 C 0.6355(4) 0.6063(3) 0.4866(2) 0.0671(12) Uani 1 1 d . . . H31A H 0.6492 0.6706 0.5192 0.081 Uiso 1 1 calc R . . C32 C 0.5658(4) 0.5897(3) 0.4161(3) 0.0705(12) Uani 1 1 d . . . H32A H 0.5315 0.6424 0.4014 0.085 Uiso 1 1 calc R . . C33 C 0.5467(4) 0.4939(2) 0.3669(2) 0.0550(9) Uani 1 1 d . . . H33A H 0.5013 0.4831 0.3190 0.066 Uiso 1 1 calc R . . C34 C 0.4071(3) 0.2360(2) 0.33299(16) 0.0329(7) Uani 1 1 d . . . C35 C 0.3043(3) 0.2735(2) 0.30282(19) 0.0448(8) Uani 1 1 d . . . H35A H 0.3143 0.3225 0.2763 0.054 Uiso 1 1 calc R . . C36 C 0.1860(3) 0.2375(3) 0.3124(2) 0.0530(9) Uani 1 1 d . . . H36A H 0.1175 0.2627 0.2923 0.064 Uiso 1 1 calc R . . C37 C 0.1704(3) 0.1647(3) 0.3515(2) 0.0537(10) Uani 1 1 d . . . H37A H 0.0916 0.1410 0.3578 0.064 Uiso 1 1 calc R . . C38 C 0.2718(3) 0.1274(2) 0.38107(19) 0.0474(8) Uani 1 1 d . . . H38A H 0.2610 0.0776 0.4068 0.057 Uiso 1 1 calc R . . C39 C 0.3903(3) 0.1634(2) 0.37282(17) 0.0378(7) Uani 1 1 d . . . H39A H 0.4585 0.1389 0.3940 0.045 Uiso 1 1 calc R . . C40 C 0.9988(4) 0.2892(5) 0.5067(4) 0.135(3) Uani 1 1 d . . . H40A H 1.0407 0.3058 0.4693 0.162 Uiso 1 1 calc R . . H40B H 1.0207 0.2256 0.5151 0.162 Uiso 1 1 calc R . . C41 C 1.0453(5) 0.3661(5) 0.5720(3) 0.133(3) Uani 1 1 d . . . H41A H 1.1307 0.3631 0.5909 0.199 Uiso 1 1 calc R . . H41B H 0.9971 0.3563 0.6077 0.199 Uiso 1 1 calc R . . H41C H 1.0401 0.4317 0.5622 0.199 Uiso 1 1 calc R . . C42 C 0.6964(4) 0.1771(4) 0.5497(2) 0.0794(14) Uani 1 1 d . . . H42A H 0.7586 0.1361 0.5615 0.095 Uiso 1 1 calc R . . H42B H 0.7293 0.2476 0.5768 0.095 Uiso 1 1 calc R . . C43 C 0.5825(4) 0.1412(3) 0.5715(2) 0.0727(12) Uani 1 1 d . . . H43A H 0.5987 0.1521 0.6241 0.109 Uiso 1 1 calc R . . H43B H 0.5548 0.0695 0.5485 0.109 Uiso 1 1 calc R . . H43C H 0.5190 0.1783 0.5563 0.109 Uiso 1 1 calc R . . C44 C 0.7948(5) -0.0192(3) 0.4094(3) 0.0927(17) Uani 1 1 d . . . H44A H 0.7067 -0.0260 0.4096 0.111 Uiso 1 1 calc R . . H44B H 0.8021 -0.0376 0.3584 0.111 Uiso 1 1 calc R . . C45 C 0.8436(6) -0.0882(4) 0.4442(3) 0.120(2) Uani 1 1 d . . . H45A H 0.7941 -0.1551 0.4227 0.180 Uiso 1 1 calc R . . H45B H 0.8430 -0.0681 0.4957 0.180 Uiso 1 1 calc R . . H45C H 0.9277 -0.0894 0.4385 0.180 Uiso 1 1 calc R . . O999 O 0.2200(5) 0.6725(3) 0.2781(3) 0.168(2) Uani 1 1 d . . . C997 C 0.1445(6) 0.5963(4) 0.2600(3) 0.0957(17) Uani 1 1 d . . . C998 C 0.0175(7) 0.5926(6) 0.2109(5) 0.174(4) Uani 1 1 d . . . H99A H -0.0105 0.6562 0.2259 0.261 Uiso 1 1 calc R . . H99B H -0.0416 0.5376 0.2156 0.261 Uiso 1 1 calc R . . H99C H 0.0249 0.5816 0.1605 0.261 Uiso 1 1 calc R . . C999 C 0.1642(6) 0.5038(5) 0.2783(4) 0.136(3) Uani 1 1 d . . . H99D H 0.2388 0.5165 0.3160 0.204 Uiso 1 1 calc R . . H99E H 0.1727 0.4550 0.2354 0.204 Uiso 1 1 calc R . . H99F H 0.0945 0.4770 0.2961 0.204 Uiso 1 1 calc R . . P5 P 0.27357(10) 0.39287(8) 0.07148(10) 0.0924(5) Uani 1 1 d . . . F1 F 0.1866(5) 0.4653(3) 0.1020(2) 0.185(2) Uani 1 1 d . . . F2 F 0.3353(4) 0.4744(2) 0.0388(2) 0.173(2) Uani 1 1 d . . . F3 F 0.3710(3) 0.4346(3) 0.1458(3) 0.186(2) Uani 1 1 d . . . F4 F 0.2181(3) 0.3099(2) 0.1111(3) 0.1630(19) Uani 1 1 d . . . F5 F 0.1746(3) 0.3479(3) 0.0024(3) 0.204(3) Uani 1 1 d . . . F6 F 0.3575(3) 0.3155(3) 0.0416(3) 0.179(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0288(2) 0.0309(2) 0.0369(3) 0.00259(19) 0.00317(19) 0.00436(18) Mn2 0.0278(2) 0.0285(2) 0.0243(2) 0.00246(17) 0.00186(17) 0.00301(17) P1 0.0296(4) 0.0275(4) 0.0235(4) 0.0023(3) 0.0043(3) 0.0047(3) P2 0.0331(4) 0.0273(4) 0.0254(4) 0.0001(3) 0.0062(3) 0.0049(3) P3 0.0378(4) 0.0450(5) 0.0284(4) 0.0058(3) -0.0024(3) 0.0046(4) O1 0.0608(16) 0.0728(17) 0.0524(16) 0.0268(13) 0.0029(13) 0.0177(13) O2 0.0552(15) 0.0487(14) 0.0561(16) 0.0028(12) 0.0066(13) -0.0169(12) O3 0.0448(13) 0.0352(12) 0.0492(14) 0.0071(10) 0.0074(11) -0.0028(10) O4 0.0670(17) 0.0714(17) 0.0450(15) 0.0198(13) -0.0032(13) 0.0254(14) O5 0.0488(14) 0.0684(15) 0.0264(11) 0.0157(10) 0.0036(10) 0.0042(11) O6 0.0506(15) 0.0693(17) 0.0510(16) 0.0055(13) -0.0163(12) -0.0073(13) N1 0.0288(13) 0.0322(13) 0.0366(14) 0.0045(11) 0.0028(11) 0.0038(10) N2 0.0402(15) 0.0375(14) 0.0443(16) 0.0108(12) 0.0079(13) 0.0113(12) N3 0.0462(17) 0.0363(15) 0.063(2) 0.0068(14) 0.0044(15) -0.0047(13) C1 0.0267(15) 0.0316(15) 0.0282(15) 0.0067(12) -0.0011(12) -0.0013(12) C2 0.045(2) 0.153(5) 0.061(3) 0.034(3) 0.022(2) 0.036(3) C3 0.061(2) 0.0465(19) 0.042(2) 0.0007(15) 0.0141(17) 0.0159(17) C4 0.050(2) 0.062(2) 0.0372(19) 0.0013(16) -0.0009(16) 0.0071(18) C5 0.057(2) 0.055(2) 0.042(2) 0.0132(16) 0.0130(17) 0.0189(18) C6 0.058(2) 0.051(2) 0.041(2) 0.0028(16) 0.0214(18) -0.0064(17) C7 0.0369(18) 0.075(2) 0.0372(19) 0.0098(17) 0.0125(15) 0.0129(17) C8 0.0425(19) 0.0328(17) 0.048(2) 0.0008(14) 0.0017(16) 0.0046(15) C9 0.043(2) 0.0376(19) 0.080(3) 0.0171(18) -0.0037(19) -0.0100(15) C10 0.119(5) 0.124(5) 0.124(5) 0.033(4) 0.042(4) -0.044(4) C11 0.060(3) 0.101(4) 0.200(7) 0.077(4) -0.040(4) -0.024(3) C12 0.072(3) 0.047(3) 0.305(10) 0.052(4) 0.033(5) 0.001(2) C13 0.0392(17) 0.0385(17) 0.0291(16) 0.0026(13) 0.0034(13) 0.0042(14) C14 0.0327(15) 0.0340(16) 0.0255(15) 0.0044(12) 0.0040(12) 0.0081(13) C15 0.0368(16) 0.0268(14) 0.0260(15) -0.0005(11) 0.0052(12) -0.0016(12) C16 0.0396(17) 0.0381(17) 0.0357(17) 0.0066(13) 0.0070(14) 0.0007(13) C17 0.0396(19) 0.059(2) 0.050(2) 0.0101(17) 0.0142(17) -0.0028(16) C18 0.065(3) 0.047(2) 0.043(2) 0.0067(16) 0.0170(19) -0.0172(18) C19 0.072(3) 0.045(2) 0.0383(19) 0.0172(15) 0.0089(18) -0.0001(18) C20 0.0466(19) 0.0371(17) 0.0337(17) 0.0070(13) 0.0060(15) 0.0045(14) C21 0.0342(16) 0.0336(15) 0.0200(14) 0.0053(11) 0.0060(12) 0.0009(12) C22 0.0439(18) 0.0363(16) 0.0294(16) 0.0049(13) 0.0059(14) 0.0039(13) C23 0.070(2) 0.0349(17) 0.0306(17) 0.0022(13) 0.0143(17) -0.0028(16) C24 0.058(2) 0.053(2) 0.0274(17) 0.0027(15) 0.0040(16) -0.0222(17) C25 0.0377(18) 0.071(2) 0.0307(17) 0.0092(16) -0.0017(14) -0.0088(17) C26 0.0387(18) 0.0474(18) 0.0303(16) 0.0088(14) 0.0045(14) 0.0021(14) C27 0.0457(18) 0.0332(15) 0.0320(16) 0.0067(12) 0.0096(14) 0.0161(13) C28 0.0375(17) 0.0304(15) 0.0383(17) -0.0037(13) 0.0156(14) -0.0020(13) C29 0.070(3) 0.046(2) 0.039(2) -0.0065(15) 0.0061(18) 0.0043(18) C30 0.086(3) 0.057(2) 0.045(2) -0.0140(18) 0.014(2) 0.000(2) C31 0.085(3) 0.041(2) 0.063(3) -0.0161(19) 0.037(2) -0.007(2) C32 0.099(3) 0.0320(19) 0.082(3) 0.0010(19) 0.036(3) 0.018(2) C33 0.074(3) 0.0363(18) 0.050(2) -0.0003(15) 0.0148(19) 0.0119(17) C34 0.0303(15) 0.0290(15) 0.0309(15) -0.0060(12) 0.0042(12) 0.0028(12) C35 0.0389(18) 0.0391(17) 0.048(2) -0.0005(15) 0.0030(15) 0.0063(14) C36 0.0326(18) 0.053(2) 0.059(2) -0.0078(18) -0.0006(16) 0.0088(15) C37 0.0355(19) 0.048(2) 0.059(2) -0.0138(17) 0.0101(17) -0.0094(15) C38 0.047(2) 0.0409(18) 0.048(2) -0.0012(15) 0.0156(17) -0.0032(15) C39 0.0351(17) 0.0360(16) 0.0370(17) -0.0009(13) 0.0082(14) 0.0052(13) C40 0.045(3) 0.129(5) 0.160(6) -0.061(4) -0.021(3) -0.002(3) C41 0.069(3) 0.165(6) 0.096(4) -0.051(4) -0.009(3) -0.035(4) C42 0.073(3) 0.132(4) 0.030(2) 0.027(2) 0.007(2) 0.003(3) C43 0.088(3) 0.089(3) 0.044(2) 0.020(2) 0.023(2) 0.010(3) C44 0.152(5) 0.055(3) 0.061(3) 0.013(2) -0.015(3) 0.035(3) C45 0.161(6) 0.095(4) 0.086(4) 0.053(3) -0.017(4) -0.030(4) O999 0.222(6) 0.096(3) 0.137(4) -0.014(3) 0.016(4) -0.034(4) C997 0.126(5) 0.065(3) 0.084(4) 0.000(3) 0.025(3) 0.005(3) C998 0.169(7) 0.172(7) 0.178(8) 0.045(6) -0.019(6) 0.097(6) C999 0.145(6) 0.133(5) 0.177(7) 0.093(5) 0.058(5) 0.067(5) P5 0.0433(6) 0.0469(6) 0.1704(15) 0.0379(8) -0.0255(8) -0.0005(5) F1 0.224(5) 0.122(3) 0.169(4) -0.017(3) -0.049(3) 0.115(3) F2 0.215(4) 0.096(2) 0.170(4) 0.095(2) -0.075(3) -0.046(3) F3 0.106(3) 0.204(4) 0.232(5) 0.157(4) -0.081(3) -0.041(3) F4 0.082(2) 0.093(2) 0.351(6) 0.085(3) 0.105(3) 0.0190(17) F5 0.105(3) 0.114(3) 0.272(5) -0.097(3) -0.088(3) 0.022(2) F6 0.123(3) 0.190(4) 0.343(7) 0.194(5) 0.138(4) 0.108(3) _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 N2 1.655(3) . ? Mn1 C8 1.922(3) . ? Mn1 N1 1.968(3) . ? Mn1 C3 2.119(3) . ? Mn1 C6 2.130(3) . ? Mn1 C7 2.133(3) . ? Mn1 C4 2.170(3) . ? Mn1 C5 2.178(4) . ? Mn2 C13 1.827(3) . ? Mn2 C14 1.829(3) . ? Mn2 C1 1.955(3) . ? Mn2 P3 2.2049(10) . ? Mn2 P1 2.2828(9) . ? Mn2 P2 2.2902(9) . ? P1 C21 1.819(3) . ? P1 C15 1.825(3) . ? P1 C27 1.833(3) . ? P1 P2 2.6956(11) . ? P2 C34 1.832(3) . ? P2 C28 1.832(3) . ? P2 C27 1.837(3) . ? P3 O5 1.593(2) . ? P3 O6 1.599(2) . ? P3 O4 1.605(3) . ? O1 N2 1.176(3) . ? O2 C13 1.149(3) . ? O3 C14 1.147(3) . ? O4 C44 1.460(5) . ? O5 C42 1.462(4) . ? O6 C40 1.361(5) . ? N1 C1 1.151(4) . ? N3 C8 1.151(4) . ? N3 C9 1.467(4) . ? C2 C7 1.496(5) . ? C3 C4 1.413(5) . ? C3 C7 1.424(5) . ? C4 C5 1.367(5) . ? C5 C6 1.416(5) . ? C6 C7 1.424(5) . ? C9 C11 1.457(6) . ? C9 C12 1.465(6) . ? C9 C10 1.543(7) . ? C15 C20 1.390(4) . ? C15 C16 1.393(4) . ? C16 C17 1.385(4) . ? C17 C18 1.378(5) . ? C18 C19 1.379(5) . ? C19 C20 1.387(5) . ? C21 C26 1.387(4) . ? C21 C22 1.402(4) . ? C22 C23 1.390(4) . ? C23 C24 1.374(5) . ? C24 C25 1.373(5) . ? C25 C26 1.405(4) . ? C28 C29 1.372(4) . ? C28 C33 1.383(5) . ? C29 C30 1.401(5) . ? C30 C31 1.350(6) . ? C31 C32 1.378(6) . ? C32 C33 1.391(5) . ? C34 C39 1.390(4) . ? C34 C35 1.394(4) . ? C35 C36 1.398(5) . ? C36 C37 1.380(5) . ? C37 C38 1.375(5) . ? C38 C39 1.391(4) . ? C40 C41 1.399(6) . ? C42 C43 1.459(6) . ? C44 C45 1.379(6) . ? O999 C997 1.186(6) . ? C997 C999 1.416(7) . ? C997 C998 1.531(8) . ? P5 F5 1.501(4) . ? P5 F2 1.536(4) . ? P5 F3 1.556(4) . ? P5 F1 1.562(4) . ? P5 F6 1.576(4) . ? P5 F4 1.612(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn1 C8 95.80(13) . . ? N2 Mn1 N1 98.30(12) . . ? C8 Mn1 N1 89.42(12) . . ? N2 Mn1 C3 109.86(13) . . ? C8 Mn1 C3 95.43(14) . . ? N1 Mn1 C3 150.71(13) . . ? N2 Mn1 C6 109.97(14) . . ? C8 Mn1 C6 151.45(14) . . ? N1 Mn1 C6 98.50(12) . . ? C3 Mn1 C6 64.89(14) . . ? N2 Mn1 C7 90.72(13) . . ? C8 Mn1 C7 132.43(14) . . ? N1 Mn1 C7 136.14(13) . . ? C3 Mn1 C7 39.13(13) . . ? C6 Mn1 C7 39.02(13) . . ? N2 Mn1 C4 148.29(14) . . ? C8 Mn1 C4 88.03(14) . . ? N1 Mn1 C4 113.24(12) . . ? C3 Mn1 C4 38.46(13) . . ? C6 Mn1 C4 63.61(14) . . ? C7 Mn1 C4 64.55(13) . . ? N2 Mn1 C5 148.31(13) . . ? C8 Mn1 C5 115.30(14) . . ? N1 Mn1 C5 88.45(12) . . ? C3 Mn1 C5 63.36(14) . . ? C6 Mn1 C5 38.35(13) . . ? C7 Mn1 C5 64.27(14) . . ? C4 Mn1 C5 36.64(13) . . ? C13 Mn2 C14 176.50(13) . . ? C13 Mn2 C1 91.38(12) . . ? C14 Mn2 C1 85.38(12) . . ? C13 Mn2 P3 89.25(10) . . ? C14 Mn2 P3 89.67(9) . . ? C1 Mn2 P3 94.37(9) . . ? C13 Mn2 P1 89.36(10) . . ? C14 Mn2 P1 92.12(9) . . ? C1 Mn2 P1 92.64(8) . . ? P3 Mn2 P1 172.88(4) . . ? C13 Mn2 P2 89.95(10) . . ? C14 Mn2 P2 93.52(9) . . ? C1 Mn2 P2 164.80(8) . . ? P3 Mn2 P2 100.78(3) . . ? P1 Mn2 P2 72.24(3) . . ? C21 P1 C15 104.10(12) . . ? C21 P1 C27 108.49(14) . . ? C15 P1 C27 105.36(13) . . ? C21 P1 Mn2 118.72(9) . . ? C15 P1 Mn2 123.01(10) . . ? C27 P1 Mn2 95.27(10) . . ? C21 P1 P2 115.71(10) . . ? C15 P1 P2 134.61(9) . . ? C27 P1 P2 42.80(9) . . ? Mn2 P1 P2 54.01(3) . . ? C34 P2 C28 102.06(13) . . ? C34 P2 C27 105.58(14) . . ? C28 P2 C27 104.36(14) . . ? C34 P2 Mn2 121.37(9) . . ? C28 P2 Mn2 125.26(11) . . ? C27 P2 Mn2 94.91(9) . . ? C34 P2 P1 114.93(9) . . ? C28 P2 P1 134.84(10) . . ? C27 P2 P1 42.68(9) . . ? Mn2 P2 P1 53.76(2) . . ? O5 P3 O6 100.60(14) . . ? O5 P3 O4 104.11(14) . . ? O6 P3 O4 98.85(14) . . ? O5 P3 Mn2 113.48(9) . . ? O6 P3 Mn2 117.37(11) . . ? O4 P3 Mn2 119.66(10) . . ? C44 O4 P3 119.7(3) . . ? C42 O5 P3 122.6(2) . . ? C40 O6 P3 132.4(3) . . ? C1 N1 Mn1 173.6(2) . . ? O1 N2 Mn1 174.4(3) . . ? C8 N3 C9 177.7(3) . . ? N1 C1 Mn2 175.0(2) . . ? C4 C3 C7 108.2(3) . . ? C4 C3 Mn1 72.7(2) . . ? C7 C3 Mn1 70.97(19) . . ? C5 C4 C3 108.6(3) . . ? C5 C4 Mn1 72.0(2) . . ? C3 C4 Mn1 68.80(19) . . ? C4 C5 C6 109.1(3) . . ? C4 C5 Mn1 71.4(2) . . ? C6 C5 Mn1 68.99(19) . . ? C5 C6 C7 107.7(3) . . ? C5 C6 Mn1 72.7(2) . . ? C7 C6 Mn1 70.58(19) . . ? C3 C7 C6 106.4(3) . . ? C3 C7 C2 127.8(4) . . ? C6 C7 C2 125.8(4) . . ? C3 C7 Mn1 69.90(19) . . ? C6 C7 Mn1 70.40(19) . . ? C2 C7 Mn1 124.6(3) . . ? N3 C8 Mn1 177.7(3) . . ? C11 C9 C12 117.5(4) . . ? C11 C9 N3 108.0(3) . . ? C12 C9 N3 108.4(3) . . ? C11 C9 C10 108.3(5) . . ? C12 C9 C10 108.0(5) . . ? N3 C9 C10 106.1(3) . . ? O2 C13 Mn2 179.7(3) . . ? O3 C14 Mn2 176.6(3) . . ? C20 C15 C16 119.6(3) . . ? C20 C15 P1 120.3(2) . . ? C16 C15 P1 120.1(2) . . ? C17 C16 C15 119.9(3) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C20 120.0(3) . . ? C19 C20 C15 120.0(3) . . ? C26 C21 C22 119.7(3) . . ? C26 C21 P1 123.3(2) . . ? C22 C21 P1 117.0(2) . . ? C23 C22 C21 119.9(3) . . ? C24 C23 C22 120.0(3) . . ? C25 C24 C23 120.8(3) . . ? C24 C25 C26 120.1(3) . . ? C21 C26 C25 119.5(3) . . ? P1 C27 P2 94.52(13) . . ? C29 C28 C33 119.1(3) . . ? C29 C28 P2 120.2(2) . . ? C33 C28 P2 120.6(3) . . ? C28 C29 C30 120.3(4) . . ? C31 C30 C29 120.4(4) . . ? C30 C31 C32 120.1(3) . . ? C31 C32 C33 120.0(4) . . ? C28 C33 C32 120.1(4) . . ? C39 C34 C35 119.2(3) . . ? C39 C34 P2 119.5(2) . . ? C35 C34 P2 121.2(2) . . ? C34 C35 C36 119.9(3) . . ? C37 C36 C35 120.4(3) . . ? C38 C37 C36 119.8(3) . . ? C37 C38 C39 120.5(3) . . ? C34 C39 C38 120.3(3) . . ? O6 C40 C41 116.3(5) . . ? C43 C42 O5 110.0(3) . . ? C45 C44 O4 115.7(4) . . ? O999 C997 C999 124.4(7) . . ? O999 C997 C998 119.9(6) . . ? C999 C997 C998 115.6(6) . . ? F5 P5 F2 92.9(3) . . ? F5 P5 F3 176.0(3) . . ? F2 P5 F3 91.11(19) . . ? F5 P5 F1 89.8(2) . . ? F2 P5 F1 91.5(3) . . ? F3 P5 F1 89.5(3) . . ? F5 P5 F6 89.6(3) . . ? F2 P5 F6 91.2(2) . . ? F3 P5 F6 90.9(3) . . ? F1 P5 F6 177.2(3) . . ? F5 P5 F4 91.5(3) . . ? F2 P5 F4 175.5(2) . . ? F3 P5 F4 84.5(2) . . ? F1 P5 F4 89.3(3) . . ? F6 P5 F4 87.98(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.701 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.066 data_cis-2[PF6] _database_code_depnum_ccdc_archive 'CCDC 644601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H59 F6 Mn2 N2 O9 P5' _chemical_formula_weight 1450.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.98(3) _cell_length_b 11.234(17) _cell_length_c 31.52(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.01(15) _cell_angle_gamma 90.00 _cell_volume 6703(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.224433 _exptl_absorpt_correction_T_max 0.881327 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 35220 _diffrn_reflns_av_R_equivalents 0.6332 _diffrn_reflns_av_sigmaI/netI 0.8120 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11793 _reflns_number_gt 2501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^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 11793 _refine_ls_number_parameters 848 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.4146 _refine_ls_R_factor_gt 0.1160 _refine_ls_wR_factor_ref 0.2848 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.874 _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 0.25933(13) 0.6496(2) 0.31630(8) 0.0296(8) Uani 1 1 d . . . C1 C 0.2751(8) 0.7287(14) 0.4145(5) 0.027(5) Uani 1 1 d . . . N1 N 0.2665(6) 0.6989(12) 0.3785(4) 0.025(4) Uani 1 1 d . . . Mn2 Mn 0.29074(14) 0.8014(2) 0.46924(8) 0.0309(8) Uani 1 1 d . . . N2 N 0.2485(8) 0.9254(14) 0.4574(4) 0.045(4) Uani 1 1 d . . . O1 O 0.2239(7) 1.0241(12) 0.4504(4) 0.060(4) Uani 1 1 d . . . C4 C 0.3871(10) 1.0184(17) 0.5085(6) 0.080(8) Uani 1 1 d . . . H4A H 0.4283 1.0333 0.5272 0.121 Uiso 1 1 calc R . . H4B H 0.3460 1.0465 0.5214 0.121 Uiso 1 1 calc R . . H4C H 0.3915 1.0592 0.4820 0.121 Uiso 1 1 calc R . . C5 C 0.3803(10) 0.8867(16) 0.5003(6) 0.043(6) Uani 1 1 d . . . C6 C 0.3507(9) 0.804(2) 0.5297(5) 0.058(7) Uani 1 1 d . . . H6A H 0.3337 0.8212 0.5577 0.069 Uiso 1 1 calc R . . C7 C 0.3569(9) 0.6869(17) 0.5093(6) 0.041(5) Uani 1 1 d . . . H7A H 0.3439 0.6096 0.5208 0.049 Uiso 1 1 calc R . . C8 C 0.3878(9) 0.7063(19) 0.4728(6) 0.044(5) Uani 1 1 d . . . H8A H 0.3990 0.6430 0.4530 0.053 Uiso 1 1 calc R . . C9 C 0.3990(9) 0.8241(19) 0.4658(5) 0.047(6) Uani 1 1 d . . . H9A H 0.4219 0.8574 0.4415 0.057 Uiso 1 1 calc R . . P4 P 0.1962(3) 0.7077(5) 0.48819(15) 0.0341(13) Uani 1 1 d . . . O4 O 0.1554(6) 0.7579(9) 0.5280(3) 0.037(3) Uani 1 1 d . . . O5 O 0.1295(5) 0.6911(10) 0.4549(3) 0.032(3) Uani 1 1 d . . . O6 O 0.2123(5) 0.5707(10) 0.4999(3) 0.036(3) Uani 1 1 d . . . C10 C 0.1861(9) 0.8299(16) 0.5615(5) 0.031(5) Uani 1 1 d . . . C11 C 0.2119(8) 0.7757(17) 0.5979(5) 0.045(5) Uani 1 1 d U . . H11A H 0.2071 0.6939 0.6011 0.053 Uiso 1 1 calc R . . C12 C 0.2464(9) 0.845(2) 0.6313(6) 0.062(6) Uani 1 1 d U . . H12A H 0.2663 0.8091 0.6560 0.075 Uiso 1 1 calc R . . C13 C 0.2489(11) 0.9668(19) 0.6254(6) 0.072(7) Uani 1 1 d . . . H13A H 0.2703 1.0139 0.6469 0.086 Uiso 1 1 calc R . . C14 C 0.2211(11) 1.0203(17) 0.5892(7) 0.059(6) Uani 1 1 d . . . H14A H 0.2226 1.1027 0.5867 0.070 Uiso 1 1 calc R . . C15 C 0.1901(8) 0.9512(17) 0.5553(6) 0.037(5) Uani 1 1 d . . . H15A H 0.1731 0.9862 0.5299 0.044 Uiso 1 1 calc R . . C16 C 0.0936(10) 0.7876(17) 0.4349(6) 0.044(5) Uani 1 1 d . . . C17 C 0.0929(9) 0.8041(16) 0.3932(6) 0.037(5) Uani 1 1 d . . . H17A H 0.1190 0.7541 0.3768 0.045 Uiso 1 1 calc R . . C18 C 0.0529(11) 0.8967(17) 0.3737(6) 0.052(6) Uani 1 1 d . . . H18A H 0.0594 0.9151 0.3454 0.063 Uiso 1 1 calc R . . C19 C 0.0052(11) 0.9602(19) 0.3944(7) 0.061(6) Uani 1 1 d . . . H19A H -0.0251 1.0150 0.3805 0.073 Uiso 1 1 calc R . . C20 C 0.0049(11) 0.9374(17) 0.4384(7) 0.063(7) Uani 1 1 d . . . H20A H -0.0259 0.9802 0.4543 0.076 Uiso 1 1 calc R . . C21 C 0.0487(8) 0.8539(17) 0.4586(5) 0.037(5) Uani 1 1 d . . . H21A H 0.0481 0.8421 0.4878 0.044 Uiso 1 1 calc R . . C22 C 0.1681(10) 0.4931(16) 0.5225(6) 0.032(5) Uani 1 1 d U . . C23 C 0.1049(9) 0.4606(16) 0.5053(6) 0.046(6) Uani 1 1 d . . . H23A H 0.0879 0.4881 0.4787 0.055 Uiso 1 1 calc R . . C24 C 0.0658(9) 0.3839(17) 0.5288(6) 0.048(6) Uani 1 1 d . . . H24A H 0.0220 0.3583 0.5173 0.057 Uiso 1 1 calc R . . C25 C 0.0903(10) 0.3426(15) 0.5702(6) 0.039(5) Uani 1 1 d . . . H25A H 0.0613 0.2969 0.5864 0.047 Uiso 1 1 calc R . . C26 C 0.1567(11) 0.3716(18) 0.5854(6) 0.052(6) Uani 1 1 d . . . H26A H 0.1760 0.3409 0.6110 0.062 Uiso 1 1 calc R . . C27 C 0.1945(10) 0.4479(18) 0.5615(6) 0.049(6) Uani 1 1 d . . . H27A H 0.2396 0.4703 0.5720 0.058 Uiso 1 1 calc R . . C2 C 0.2012(9) 0.7676(16) 0.3036(5) 0.031(5) Uani 1 1 d . . . O2 O 0.1646(7) 0.8533(12) 0.2968(4) 0.067(4) Uani 1 1 d . . . C3 C 0.2567(8) 0.6205(14) 0.2624(5) 0.025(4) Uani 1 1 d U . . O3 O 0.2595(6) 0.5979(11) 0.2254(3) 0.057(4) Uani 1 1 d . . . P1 P 0.3569(2) 0.7645(4) 0.30856(14) 0.0293(13) Uani 1 1 d . . . P2 P 0.3582(2) 0.5282(4) 0.33104(13) 0.0287(13) Uani 1 1 d . . . P3 P 0.1799(3) 0.5090(5) 0.32364(15) 0.0364(14) Uani 1 1 d . . . O7 O 0.1096(5) 0.5019(10) 0.2916(3) 0.036(3) Uani 1 1 d . . . O8 O 0.1520(5) 0.5083(10) 0.3710(3) 0.034(3) Uani 1 1 d . . . O9 O 0.2042(5) 0.3712(10) 0.3204(4) 0.041(3) Uani 1 1 d . . . C28 C 0.0803(9) 0.5998(18) 0.2668(6) 0.037(5) Uani 1 1 d . . . C29 C 0.0934(10) 0.6011(19) 0.2241(7) 0.061(7) Uani 1 1 d . . . H29A H 0.1191 0.5411 0.2120 0.073 Uiso 1 1 calc R . . C30 C 0.0660(12) 0.698(2) 0.2003(7) 0.069(7) Uani 1 1 d . . . H30A H 0.0772 0.7066 0.1722 0.083 Uiso 1 1 calc R . . C31 C 0.0238(11) 0.779(2) 0.2172(9) 0.078(8) Uani 1 1 d . . . H31A H 0.0048 0.8411 0.2007 0.094 Uiso 1 1 calc R . . C32 C 0.0091(11) 0.769(2) 0.2585(7) 0.066(7) Uani 1 1 d . . . H32A H -0.0219 0.8231 0.2695 0.079 Uiso 1 1 calc R . . C33 C 0.0392(11) 0.6793(17) 0.2852(7) 0.061(7) Uani 1 1 d . . . H33A H 0.0311 0.6753 0.3139 0.073 Uiso 1 1 calc R . . C34 C 0.1036(10) 0.4278(19) 0.3858(6) 0.043(5) Uani 1 1 d . . . C35 C 0.0338(9) 0.4576(16) 0.3861(5) 0.033(5) Uani 1 1 d U . . H35A H 0.0182 0.5307 0.3752 0.040 Uiso 1 1 calc R . . C36 C -0.0138(9) 0.380(2) 0.4024(6) 0.056(6) Uani 1 1 d . . . H36A H -0.0616 0.3987 0.4015 0.067 Uiso 1 1 calc R . . C37 C 0.0102(12) 0.2748(19) 0.4199(6) 0.053(6) Uani 1 1 d . . . H37A H -0.0209 0.2232 0.4322 0.063 Uiso 1 1 calc R . . C38 C 0.0807(13) 0.2457(18) 0.4193(5) 0.057(6) Uani 1 1 d . . . H38A H 0.0963 0.1732 0.4307 0.068 Uiso 1 1 calc R . . C39 C 0.1287(10) 0.3209(18) 0.4024(5) 0.047(6) Uani 1 1 d . . . H39A H 0.1761 0.3005 0.4021 0.056 Uiso 1 1 calc R . . C40 C 0.1857(9) 0.2909(18) 0.2849(6) 0.040(5) Uani 1 1 d . . . C41 C 0.2087(9) 0.3127(18) 0.2453(6) 0.054(6) Uani 1 1 d . . . H41A H 0.2320 0.3834 0.2401 0.064 Uiso 1 1 calc R . . C42 C 0.1968(9) 0.226(2) 0.2121(7) 0.073(8) Uani 1 1 d . . . H42A H 0.2143 0.2353 0.1854 0.088 Uiso 1 1 calc R . . C43 C 0.1588(10) 0.132(2) 0.2225(7) 0.068(7) Uani 1 1 d U . . H43A H 0.1470 0.0776 0.2010 0.081 Uiso 1 1 calc R . . C44 C 0.1365(10) 0.1098(19) 0.2599(6) 0.059(6) Uani 1 1 d U . . H44A H 0.1102 0.0413 0.2638 0.071 Uiso 1 1 calc R . . C45 C 0.1518(10) 0.1888(17) 0.2954(6) 0.056(6) Uani 1 1 d . . . H45A H 0.1397 0.1719 0.3228 0.067 Uiso 1 1 calc R . . C46 C 0.4245(8) 0.6496(14) 0.3257(5) 0.032(5) Uani 1 1 d . . . H46A H 0.4571 0.6329 0.3041 0.039 Uiso 1 1 calc R . . H46B H 0.4502 0.6691 0.3525 0.039 Uiso 1 1 calc R . . C47 C 0.3843(9) 0.8921(15) 0.3420(5) 0.031(5) Uani 1 1 d U . . C48 C 0.3306(8) 0.9667(16) 0.3578(5) 0.040(5) Uani 1 1 d . . . H48A H 0.2832 0.9485 0.3517 0.048 Uiso 1 1 calc R . . C49 C 0.3497(10) 1.0665(18) 0.3822(5) 0.044(6) Uani 1 1 d . . . H49A H 0.3158 1.1158 0.3929 0.053 Uiso 1 1 calc R . . C50 C 0.4228(11) 1.0898(17) 0.3901(5) 0.052(6) Uani 1 1 d . . . H50A H 0.4362 1.1568 0.4059 0.062 Uiso 1 1 calc R . . C51 C 0.4749(10) 1.0192(16) 0.3756(5) 0.040(5) Uani 1 1 d U . . H51A H 0.5226 1.0354 0.3817 0.047 Uiso 1 1 calc R . . C52 C 0.4519(8) 0.9225(15) 0.3514(4) 0.031(5) Uani 1 1 d U . . H52A H 0.4863 0.8742 0.3407 0.038 Uiso 1 1 calc R . . C53 C 0.3696(11) 0.8135(16) 0.2555(5) 0.037(5) Uani 1 1 d . . . C54 C 0.4225(10) 0.7810(16) 0.2312(5) 0.044(6) Uani 1 1 d . . . H54A H 0.4566 0.7304 0.2439 0.053 Uiso 1 1 calc R . . C55 C 0.4318(9) 0.8144(19) 0.1896(6) 0.051(6) Uani 1 1 d . . . H55A H 0.4691 0.7847 0.1751 0.061 Uiso 1 1 calc R . . C56 C 0.3821(11) 0.8959(18) 0.1699(6) 0.053(6) Uani 1 1 d . . . H56A H 0.3865 0.9239 0.1424 0.064 Uiso 1 1 calc R . . C57 C 0.3277(12) 0.9312(17) 0.1933(6) 0.059(7) Uani 1 1 d . . . H57A H 0.2928 0.9806 0.1808 0.071 Uiso 1 1 calc R . . C58 C 0.3230(10) 0.8950(15) 0.2353(5) 0.042(5) Uani 1 1 d . . . H58A H 0.2872 0.9266 0.2506 0.050 Uiso 1 1 calc R . . C59 C 0.3806(8) 0.4665(14) 0.3838(4) 0.022(4) Uani 1 1 d U . . C60 C 0.3299(8) 0.4310(15) 0.4107(5) 0.028(5) Uani 1 1 d . . . H60A H 0.2823 0.4395 0.4021 0.033 Uiso 1 1 calc R . . C61 C 0.3499(11) 0.3823(15) 0.4508(5) 0.040(5) Uani 1 1 d . . . H61A H 0.3153 0.3579 0.4683 0.049 Uiso 1 1 calc R . . C62 C 0.4193(9) 0.3705(15) 0.4642(5) 0.031(5) Uani 1 1 d . . . H62A H 0.4323 0.3365 0.4905 0.037 Uiso 1 1 calc R . . C63 C 0.4698(9) 0.4093(14) 0.4385(5) 0.031(5) Uani 1 1 d . . . H63A H 0.5174 0.4060 0.4477 0.037 Uiso 1 1 calc R . . C64 C 0.4492(8) 0.4532(13) 0.3987(5) 0.023(4) Uani 1 1 d U . . H64A H 0.4843 0.4751 0.3811 0.027 Uiso 1 1 calc R . . C65 C 0.3775(8) 0.4112(16) 0.2936(5) 0.030(5) Uani 1 1 d U . . C66 C 0.3892(8) 0.4383(16) 0.2520(5) 0.035(5) Uani 1 1 d . . . H66A H 0.3929 0.5174 0.2438 0.043 Uiso 1 1 calc R . . C67 C 0.3956(10) 0.3468(19) 0.2217(6) 0.061(6) Uani 1 1 d . . . H67A H 0.4019 0.3656 0.1935 0.074 Uiso 1 1 calc R . . C68 C 0.3923(9) 0.2284(16) 0.2344(5) 0.038(5) Uani 1 1 d . . . H68A H 0.3981 0.1673 0.2151 0.046 Uiso 1 1 calc R . . C69 C 0.3804(9) 0.2038(16) 0.2753(6) 0.042(5) Uani 1 1 d . . . H69A H 0.3770 0.1245 0.2834 0.051 Uiso 1 1 calc R . . C70 C 0.3730(8) 0.2924(17) 0.3062(5) 0.039(5) Uani 1 1 d . . . H70A H 0.3653 0.2725 0.3342 0.047 Uiso 1 1 calc R . . P5 P 0.6195(3) 0.7027(5) 0.40500(15) 0.0348(13) Uani 1 1 d . . . F1 F 0.5512(5) 0.7226(9) 0.4293(3) 0.058(3) Uani 1 1 d . . . F2 F 0.6874(5) 0.6850(8) 0.3791(3) 0.049(3) Uani 1 1 d . . . F3 F 0.6664(5) 0.7374(9) 0.4464(3) 0.056(3) Uani 1 1 d . . . F4 F 0.6153(5) 0.8399(8) 0.3906(3) 0.050(3) Uani 1 1 d . . . F5 F 0.5710(4) 0.6678(8) 0.3629(3) 0.040(3) Uani 1 1 d . . . F6 F 0.6241(5) 0.5649(8) 0.4197(3) 0.050(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0343(18) 0.0249(18) 0.0296(17) 0.0049(13) 0.0023(14) 0.0020(15) C1 0.036(12) 0.019(12) 0.028(11) -0.001(9) 0.002(10) 0.014(9) N1 0.021(9) 0.024(9) 0.030(9) 0.013(8) 0.006(7) 0.015(7) Mn2 0.0356(18) 0.0235(19) 0.0333(17) 0.0003(14) 0.0009(14) 0.0003(15) N2 0.050(11) 0.026(11) 0.061(11) 0.009(9) 0.007(9) -0.022(9) O1 0.073(11) 0.023(10) 0.085(11) 0.012(8) 0.007(8) 0.011(8) C4 0.097(19) 0.043(17) 0.098(18) -0.051(14) -0.016(15) 0.009(14) C5 0.085(17) 0.015(13) 0.028(12) -0.004(10) 0.010(12) -0.006(11) C6 0.039(13) 0.12(2) 0.013(11) -0.008(14) -0.001(10) 0.005(14) C7 0.050(14) 0.025(14) 0.048(13) 0.017(11) 0.004(11) -0.020(11) C8 0.039(13) 0.041(16) 0.053(14) -0.006(12) 0.001(11) -0.001(12) C9 0.051(14) 0.058(18) 0.028(12) 0.012(12) -0.024(11) 0.022(13) P4 0.042(4) 0.027(3) 0.033(3) 0.003(3) 0.004(3) 0.002(3) O4 0.046(8) 0.020(8) 0.045(8) 0.001(6) 0.008(7) 0.002(6) O5 0.030(8) 0.015(8) 0.049(8) 0.009(6) -0.007(6) 0.010(6) O6 0.046(8) 0.017(8) 0.047(8) 0.015(6) 0.012(7) 0.012(6) C10 0.038(13) 0.025(14) 0.029(11) 0.008(10) -0.006(10) 0.002(10) C11 0.045(5) 0.045(5) 0.044(5) 0.0001(10) 0.0032(11) 0.0000(10) C12 0.063(6) 0.062(6) 0.062(6) 0.0002(10) 0.0043(11) 0.0001(10) C13 0.13(2) 0.044(17) 0.042(14) -0.040(12) -0.021(14) 0.019(15) C14 0.099(19) 0.009(13) 0.070(16) -0.007(12) 0.011(15) -0.011(12) C15 0.041(14) 0.029(14) 0.045(13) 0.004(11) 0.027(11) 0.014(10) C16 0.061(15) 0.024(13) 0.049(14) -0.024(12) 0.020(13) -0.013(11) C17 0.052(14) 0.014(12) 0.047(13) -0.007(11) 0.011(11) -0.019(11) C18 0.082(18) 0.022(14) 0.054(14) 0.013(11) 0.010(13) 0.017(12) C19 0.067(17) 0.047(17) 0.067(17) 0.016(13) -0.005(14) 0.012(13) C20 0.085(19) 0.018(14) 0.086(18) 0.012(13) 0.001(15) -0.002(12) C21 0.041(13) 0.041(14) 0.027(11) 0.010(10) -0.002(10) 0.014(11) C22 0.032(5) 0.032(5) 0.032(5) 0.0002(10) 0.0025(11) 0.0000(10) C23 0.034(13) 0.027(13) 0.072(14) 0.010(11) -0.027(12) -0.026(10) C24 0.043(14) 0.044(16) 0.056(15) -0.018(12) 0.006(12) -0.012(11) C25 0.036(13) 0.032(13) 0.051(14) 0.022(10) 0.010(11) -0.006(10) C26 0.046(15) 0.048(16) 0.062(15) 0.003(12) 0.005(13) 0.001(12) C27 0.043(14) 0.050(16) 0.052(14) -0.016(12) 0.000(12) 0.004(12) C2 0.029(12) 0.025(13) 0.037(12) 0.009(10) -0.004(10) -0.006(10) O2 0.067(11) 0.034(10) 0.102(12) 0.029(9) 0.011(9) -0.007(8) C3 0.013(7) 0.028(8) 0.032(8) 0.005(7) -0.006(7) -0.004(7) O3 0.078(10) 0.072(11) 0.021(7) 0.010(7) 0.012(7) 0.012(8) P1 0.032(3) 0.021(3) 0.034(3) 0.001(2) 0.000(3) -0.003(2) P2 0.042(3) 0.022(3) 0.022(3) -0.003(2) 0.000(2) -0.002(3) P3 0.040(3) 0.031(4) 0.039(3) -0.002(3) 0.009(3) -0.006(3) O7 0.027(7) 0.033(9) 0.048(8) -0.007(6) -0.012(7) -0.010(6) O8 0.034(8) 0.029(8) 0.040(8) -0.006(6) 0.001(6) -0.011(6) O9 0.030(8) 0.019(8) 0.072(9) -0.007(7) -0.001(7) -0.003(6) C28 0.043(14) 0.039(15) 0.028(12) 0.017(11) -0.013(11) 0.007(11) C29 0.075(17) 0.051(17) 0.055(16) 0.012(13) -0.015(14) -0.013(13) C30 0.073(19) 0.08(2) 0.059(16) 0.032(16) -0.003(14) -0.011(16) C31 0.053(18) 0.061(19) 0.11(2) 0.019(18) -0.045(17) 0.030(14) C32 0.049(16) 0.08(2) 0.069(18) 0.016(16) -0.009(14) 0.004(14) C33 0.093(19) 0.016(14) 0.072(16) -0.001(12) -0.006(15) 0.014(12) C34 0.049(16) 0.033(15) 0.047(13) -0.023(11) 0.010(12) -0.005(12) C35 0.033(5) 0.033(5) 0.034(5) 0.0001(10) 0.0026(11) 0.0000(10) C36 0.023(12) 0.08(2) 0.067(15) 0.005(14) 0.026(11) -0.019(13) C37 0.069(18) 0.056(18) 0.034(13) 0.000(12) 0.006(13) -0.009(14) C38 0.095(19) 0.035(15) 0.043(14) 0.023(11) 0.022(14) 0.000(14) C39 0.040(14) 0.044(17) 0.058(14) 0.017(12) 0.013(11) -0.002(12) C40 0.026(12) 0.031(14) 0.062(15) -0.015(12) 0.002(11) -0.002(10) C41 0.071(16) 0.041(16) 0.051(14) -0.014(12) 0.022(13) -0.028(12) C42 0.034(14) 0.11(2) 0.081(17) -0.012(16) 0.040(12) -0.027(14) C43 0.068(7) 0.068(7) 0.068(7) -0.0003(10) 0.0048(11) 0.0001(10) C44 0.059(6) 0.059(6) 0.059(6) 0.0000(10) 0.0040(11) 0.0000(10) C45 0.072(16) 0.026(14) 0.067(15) 0.030(12) -0.006(12) 0.016(12) C46 0.033(11) 0.022(12) 0.043(11) -0.001(9) 0.009(9) -0.005(9) C47 0.032(5) 0.031(5) 0.031(5) -0.0001(10) 0.0024(11) 0.0001(10) C48 0.010(11) 0.037(14) 0.072(14) -0.004(11) 0.001(10) -0.016(10) C49 0.042(15) 0.045(16) 0.045(13) 0.028(11) 0.007(12) 0.008(12) C50 0.077(17) 0.041(15) 0.038(13) 0.008(10) 0.006(13) -0.019(13) C51 0.040(5) 0.039(5) 0.040(5) 0.0002(10) 0.0028(11) 0.0001(10) C52 0.033(8) 0.033(9) 0.028(8) 0.002(7) -0.003(7) -0.006(7) C53 0.071(16) 0.011(12) 0.032(12) 0.000(10) 0.016(11) -0.006(11) C54 0.058(15) 0.045(15) 0.028(12) 0.015(11) -0.017(11) -0.031(12) C55 0.031(13) 0.082(19) 0.043(13) 0.021(13) 0.016(11) -0.005(12) C56 0.059(16) 0.049(17) 0.053(15) 0.023(12) 0.018(13) -0.032(13) C57 0.11(2) 0.039(15) 0.026(13) 0.002(11) -0.002(14) -0.018(14) C58 0.072(16) 0.020(13) 0.037(13) -0.003(10) 0.027(11) 0.007(11) C59 0.026(8) 0.017(8) 0.024(7) 0.003(6) 0.008(7) 0.002(7) C60 0.019(11) 0.039(13) 0.025(11) -0.003(9) 0.001(9) 0.002(9) C61 0.067(16) 0.021(13) 0.034(13) 0.016(9) 0.006(12) -0.003(11) C62 0.041(13) 0.042(13) 0.011(10) 0.000(9) -0.003(10) 0.015(11) C63 0.034(12) 0.025(12) 0.035(12) 0.000(9) 0.015(10) 0.002(9) C64 0.023(4) 0.022(4) 0.023(4) 0.0003(10) 0.0015(11) -0.0001(10) C65 0.040(8) 0.017(8) 0.033(8) -0.009(7) 0.001(7) 0.001(7) C66 0.053(14) 0.016(12) 0.037(12) 0.009(10) 0.001(11) -0.015(10) C67 0.099(18) 0.024(14) 0.061(15) 0.014(12) 0.007(13) -0.021(13) C68 0.060(14) 0.024(14) 0.031(12) -0.017(10) 0.007(11) -0.007(11) C69 0.067(14) 0.010(11) 0.051(13) -0.012(11) 0.011(12) -0.006(10) C70 0.069(14) 0.037(14) 0.013(10) -0.006(10) 0.021(10) 0.008(11) P5 0.047(4) 0.020(3) 0.037(3) -0.003(3) 0.002(3) -0.001(3) F1 0.057(7) 0.045(8) 0.075(8) 0.031(6) 0.032(6) 0.020(6) F2 0.051(7) 0.038(8) 0.058(7) 0.009(6) 0.017(6) 0.009(6) F3 0.079(8) 0.044(8) 0.042(6) -0.004(5) -0.014(6) 0.011(6) F4 0.058(7) 0.029(7) 0.060(7) 0.013(5) -0.014(6) 0.001(6) F5 0.045(6) 0.040(7) 0.035(6) 0.013(5) -0.010(5) -0.007(5) F6 0.082(8) 0.024(7) 0.045(6) 0.009(5) 0.007(6) 0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C3 1.727(17) . ? Mn1 C2 1.753(19) . ? Mn1 N1 2.033(14) . ? Mn1 P3 2.207(6) . ? Mn1 P1 2.285(6) . ? Mn1 P2 2.340(6) . ? C1 N1 1.184(16) . ? C1 Mn2 1.912(17) . ? Mn2 N2 1.637(17) . ? Mn2 C9 2.081(19) . ? Mn2 C8 2.126(18) . ? Mn2 C5 2.129(19) . ? Mn2 C7 2.145(17) . ? Mn2 C6 2.150(16) . ? Mn2 P4 2.198(6) . ? N2 O1 1.218(17) . ? C4 C5 1.50(2) . ? C5 C9 1.36(2) . ? C5 C6 1.45(2) . ? C6 C7 1.47(2) . ? C7 C8 1.34(2) . ? C8 C9 1.36(2) . ? P4 O5 1.599(11) . ? P4 O6 1.607(11) . ? P4 O4 1.621(11) . ? O4 C10 1.420(18) . ? O5 C16 1.40(2) . ? O6 C22 1.433(18) . ? C10 C11 1.36(2) . ? C10 C15 1.38(2) . ? C11 C12 1.43(2) . ? C12 C13 1.39(2) . ? C13 C14 1.36(2) . ? C14 C15 1.41(2) . ? C16 C17 1.33(2) . ? C16 C21 1.39(2) . ? C17 C18 1.40(2) . ? C18 C19 1.36(2) . ? C19 C20 1.41(2) . ? C20 C21 1.38(2) . ? C22 C23 1.333(19) . ? C22 C27 1.39(2) . ? C23 C24 1.39(2) . ? C24 C25 1.43(2) . ? C25 C26 1.36(2) . ? C26 C27 1.37(2) . ? C2 O2 1.197(18) . ? C3 O3 1.199(16) . ? P1 C53 1.791(17) . ? P1 C47 1.832(17) . ? P1 C46 1.873(16) . ? P2 C65 1.820(16) . ? P2 C59 1.823(15) . ? P2 C46 1.870(15) . ? P3 O8 1.617(11) . ? P3 O7 1.617(11) . ? P3 O9 1.621(12) . ? O7 C28 1.437(19) . ? O8 C34 1.39(2) . ? O9 C40 1.462(19) . ? C28 C33 1.34(2) . ? C28 C29 1.39(2) . ? C29 C30 1.40(2) . ? C30 C31 1.35(3) . ? C31 C32 1.35(3) . ? C32 C33 1.41(2) . ? C34 C35 1.37(2) . ? C34 C39 1.38(2) . ? C35 C36 1.38(2) . ? C36 C37 1.37(2) . ? C37 C38 1.38(2) . ? C38 C39 1.38(2) . ? C40 C45 1.37(2) . ? C40 C41 1.37(2) . ? C41 C42 1.43(2) . ? C42 C43 1.33(2) . ? C43 C44 1.31(2) . ? C44 C45 1.44(2) . ? C47 C52 1.342(19) . ? C47 C48 1.44(2) . ? C48 C49 1.39(2) . ? C49 C50 1.42(2) . ? C50 C51 1.37(2) . ? C51 C52 1.38(2) . ? C53 C54 1.36(2) . ? C53 C58 1.40(2) . ? C54 C55 1.39(2) . ? C55 C56 1.43(2) . ? C56 C57 1.37(2) . ? C57 C58 1.39(2) . ? C59 C64 1.363(18) . ? C59 C60 1.385(18) . ? C60 C61 1.405(19) . ? C61 C62 1.36(2) . ? C62 C63 1.369(19) . ? C63 C64 1.377(18) . ? C65 C66 1.379(19) . ? C65 C70 1.40(2) . ? C66 C67 1.41(2) . ? C67 C68 1.39(2) . ? C68 C69 1.35(2) . ? C69 C70 1.41(2) . ? P5 F1 1.567(10) . ? P5 F3 1.576(10) . ? P5 F2 1.584(10) . ? P5 F4 1.607(10) . ? P5 F5 1.611(9) . ? P5 F6 1.617(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mn1 C2 86.8(8) . . ? C3 Mn1 N1 174.6(7) . . ? C2 Mn1 N1 90.7(7) . . ? C3 Mn1 P3 89.7(5) . . ? C2 Mn1 P3 98.1(6) . . ? N1 Mn1 P3 95.4(4) . . ? C3 Mn1 P1 88.3(5) . . ? C2 Mn1 P1 92.9(6) . . ? N1 Mn1 P1 87.1(4) . . ? P3 Mn1 P1 168.7(2) . . ? C3 Mn1 P2 93.0(5) . . ? C2 Mn1 P2 165.7(6) . . ? N1 Mn1 P2 88.2(4) . . ? P3 Mn1 P2 96.1(2) . . ? P1 Mn1 P2 72.9(2) . . ? N1 C1 Mn2 171.1(15) . . ? C1 N1 Mn1 175.8(13) . . ? N2 Mn2 C1 96.6(7) . . ? N2 Mn2 C9 110.7(8) . . ? C1 Mn2 C9 95.5(7) . . ? N2 Mn2 C8 148.0(8) . . ? C1 Mn2 C8 85.0(7) . . ? C9 Mn2 C8 37.8(6) . . ? N2 Mn2 C5 94.8(7) . . ? C1 Mn2 C5 132.5(7) . . ? C9 Mn2 C5 37.8(6) . . ? C8 Mn2 C5 62.7(7) . . ? N2 Mn2 C7 154.4(8) . . ? C1 Mn2 C7 108.8(7) . . ? C9 Mn2 C7 64.2(7) . . ? C8 Mn2 C7 36.7(6) . . ? C5 Mn2 C7 65.4(7) . . ? N2 Mn2 C6 114.3(8) . . ? C1 Mn2 C6 147.5(8) . . ? C9 Mn2 C6 65.3(7) . . ? C8 Mn2 C6 63.6(7) . . ? C5 Mn2 C6 39.7(6) . . ? C7 Mn2 C6 40.1(6) . . ? N2 Mn2 P4 94.2(5) . . ? C1 Mn2 P4 87.9(5) . . ? C9 Mn2 P4 154.2(6) . . ? C8 Mn2 P4 117.7(6) . . ? C5 Mn2 P4 137.0(5) . . ? C7 Mn2 P4 90.5(5) . . ? C6 Mn2 P4 99.0(6) . . ? O1 N2 Mn2 172.7(14) . . ? C9 C5 C6 108.2(18) . . ? C9 C5 C4 128.2(19) . . ? C6 C5 C4 123.6(19) . . ? C9 C5 Mn2 69.2(11) . . ? C6 C5 Mn2 70.9(10) . . ? C4 C5 Mn2 125.3(14) . . ? C5 C6 C7 104.3(15) . . ? C5 C6 Mn2 69.3(10) . . ? C7 C6 Mn2 69.8(9) . . ? C8 C7 C6 106.4(16) . . ? C8 C7 Mn2 70.9(11) . . ? C6 C7 Mn2 70.2(10) . . ? C7 C8 C9 112.3(19) . . ? C7 C8 Mn2 72.4(11) . . ? C9 C8 Mn2 69.3(12) . . ? C8 C9 C5 108.6(18) . . ? C8 C9 Mn2 72.9(12) . . ? C5 C9 Mn2 73.0(12) . . ? O5 P4 O6 99.7(6) . . ? O5 P4 O4 98.6(6) . . ? O6 P4 O4 104.4(6) . . ? O5 P4 Mn2 120.1(4) . . ? O6 P4 Mn2 112.1(5) . . ? O4 P4 Mn2 119.1(5) . . ? C10 O4 P4 125.4(10) . . ? C16 O5 P4 122.8(11) . . ? C22 O6 P4 126.0(10) . . ? C11 C10 C15 122.7(18) . . ? C11 C10 O4 118.5(17) . . ? C15 C10 O4 118.7(15) . . ? C10 C11 C12 120.0(19) . . ? C13 C12 C11 117.1(18) . . ? C14 C13 C12 122.3(19) . . ? C13 C14 C15 120.4(19) . . ? C10 C15 C14 117.4(17) . . ? C17 C16 C21 120(2) . . ? C17 C16 O5 121.5(17) . . ? C21 C16 O5 118.0(17) . . ? C16 C17 C18 120.4(19) . . ? C19 C18 C17 123(2) . . ? C18 C19 C20 115(2) . . ? C21 C20 C19 122(2) . . ? C20 C21 C16 119.3(18) . . ? C23 C22 C27 121.2(19) . . ? C23 C22 O6 120.3(17) . . ? C27 C22 O6 118.4(17) . . ? C22 C23 C24 116.9(18) . . ? C23 C24 C25 122.5(18) . . ? C26 C25 C24 118.5(18) . . ? C25 C26 C27 117.7(19) . . ? C26 C27 C22 122.8(19) . . ? O2 C2 Mn1 175.3(17) . . ? O3 C3 Mn1 175.5(14) . . ? C53 P1 C47 104.2(8) . . ? C53 P1 C46 110.3(8) . . ? C47 P1 C46 102.2(7) . . ? C53 P1 Mn1 115.8(6) . . ? C47 P1 Mn1 125.5(6) . . ? C46 P1 Mn1 97.1(5) . . ? C65 P2 C59 105.7(8) . . ? C65 P2 C46 107.6(8) . . ? C59 P2 C46 104.1(7) . . ? C65 P2 Mn1 119.1(6) . . ? C59 P2 Mn1 122.4(5) . . ? C46 P2 Mn1 95.3(5) . . ? O8 P3 O7 105.5(6) . . ? O8 P3 O9 99.5(6) . . ? O7 P3 O9 98.0(6) . . ? O8 P3 Mn1 111.7(5) . . ? O7 P3 Mn1 120.6(5) . . ? O9 P3 Mn1 118.5(5) . . ? C28 O7 P3 124.9(11) . . ? C34 O8 P3 125.3(10) . . ? C40 O9 P3 125.7(11) . . ? C33 C28 C29 124.1(19) . . ? C33 C28 O7 119.3(18) . . ? C29 C28 O7 116.5(19) . . ? C28 C29 C30 116(2) . . ? C31 C30 C29 121(2) . . ? C30 C31 C32 120(2) . . ? C31 C32 C33 122(2) . . ? C28 C33 C32 116(2) . . ? C35 C34 C39 121.3(19) . . ? C35 C34 O8 120.4(19) . . ? C39 C34 O8 118.2(17) . . ? C34 C35 C36 120.4(19) . . ? C37 C36 C35 119.3(19) . . ? C36 C37 C38 120(2) . . ? C39 C38 C37 122(2) . . ? C38 C39 C34 117.4(19) . . ? C45 C40 C41 123.7(19) . . ? C45 C40 O9 115.1(18) . . ? C41 C40 O9 120.8(17) . . ? C40 C41 C42 120.0(19) . . ? C43 C42 C41 114.7(19) . . ? C44 C43 C42 126(2) . . ? C43 C44 C45 121(2) . . ? C40 C45 C44 113.7(18) . . ? P2 C46 P1 94.4(7) . . ? C52 C47 C48 117.7(16) . . ? C52 C47 P1 123.7(14) . . ? C48 C47 P1 118.5(13) . . ? C49 C48 C47 119.9(16) . . ? C48 C49 C50 117.3(18) . . ? C51 C50 C49 123.8(19) . . ? C50 C51 C52 115.6(18) . . ? C47 C52 C51 125.7(18) . . ? C54 C53 C58 112.9(16) . . ? C54 C53 P1 126.7(16) . . ? C58 C53 P1 120.4(15) . . ? C53 C54 C55 127.6(19) . . ? C54 C55 C56 117.4(18) . . ? C57 C56 C55 116.9(18) . . ? C56 C57 C58 122(2) . . ? C57 C58 C53 123.0(18) . . ? C64 C59 C60 116.4(14) . . ? C64 C59 P2 120.9(12) . . ? C60 C59 P2 122.7(12) . . ? C59 C60 C61 120.5(15) . . ? C62 C61 C60 120.9(17) . . ? C61 C62 C63 119.1(16) . . ? C62 C63 C64 119.2(16) . . ? C59 C64 C63 123.9(15) . . ? C66 C65 C70 119.9(15) . . ? C66 C65 P2 120.6(14) . . ? C70 C65 P2 119.1(13) . . ? C65 C66 C67 120.6(17) . . ? C68 C67 C66 119.5(18) . . ? C69 C68 C67 118.9(17) . . ? C68 C69 C70 123.1(17) . . ? C65 C70 C69 117.9(15) . . ? F1 P5 F3 89.9(6) . . ? F1 P5 F2 178.0(6) . . ? F3 P5 F2 91.5(6) . . ? F1 P5 F4 88.5(6) . . ? F3 P5 F4 90.7(6) . . ? F2 P5 F4 90.1(5) . . ? F1 P5 F5 89.5(5) . . ? F3 P5 F5 179.5(6) . . ? F2 P5 F5 89.0(5) . . ? F4 P5 F5 89.2(5) . . ? F1 P5 F6 91.5(6) . . ? F3 P5 F6 89.0(5) . . ? F2 P5 F6 89.9(5) . . ? F4 P5 F6 179.7(7) . . ? F5 P5 F6 91.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.572 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.118 #===END data_8[PF6].1.5CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 644602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H56 Cl3 F6 Mn2 N3 O6 P4' _chemical_formula_weight 1255.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9087(6) _cell_length_b 12.8321(8) _cell_length_c 22.7982(14) _cell_angle_alpha 86.824(1) _cell_angle_beta 86.597(1) _cell_angle_gamma 79.134(1) _cell_volume 2838.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 135 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735741 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24825 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9978 _reflns_number_gt 5307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^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 9978 _refine_ls_number_parameters 747 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.978 _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 1.72925(8) -0.69985(6) 0.09123(3) 0.0403(2) Uani 1 1 d . . . Mn2 Mn 1.63678(9) -0.76106(6) 0.31236(3) 0.0511(2) Uani 1 1 d . A . C1 C 1.6831(5) -0.7215(4) 0.1749(2) 0.0454(12) Uani 1 1 d . . . N1 N 1.6616(5) -0.7366(3) 0.22476(18) 0.0487(11) Uani 1 1 d . . . N2 N 1.8565(5) -0.8033(4) 0.08668(17) 0.0458(10) Uani 1 1 d . . . O1 O 1.9508(4) -0.8743(3) 0.08125(18) 0.0727(12) Uani 1 1 d . . . C2 C 1.8196(8) -0.7954(5) 0.3221(2) 0.0626(16) Uani 1 1 d . . . O2 O 1.9360(5) -0.8182(4) 0.33024(19) 0.0795(13) Uani 1 1 d . . . C3 C 1.6052(6) -0.7763(4) 0.3896(2) 0.0500(13) Uani 1 1 d . . . O3 O 1.5865(4) -0.7856(3) 0.44029(15) 0.0607(10) Uani 1 1 d . . . P1 P 1.61582(14) -0.58021(10) 0.31665(5) 0.0432(3) Uani 1 1 d . . . P3 P 1.6246(2) -0.93024(13) 0.30182(6) 0.0746(6) Uani 1 1 d D . . P2 P 1.40459(15) -0.68406(11) 0.29868(5) 0.0483(4) Uani 1 1 d . . . O4 O 1.6853(5) -0.9862(3) 0.24269(18) 0.0763(12) Uani 1 1 d . A . C5 C 1.8273(9) -0.9914(6) 0.2234(3) 0.099(2) Uani 1 1 d . . . H5A H 1.8418 -0.9193 0.2104 0.119 Uiso 1 1 calc R A . H5B H 1.8859 -1.0158 0.2570 0.119 Uiso 1 1 calc R . . C6 C 1.8680(10) -1.0600(7) 0.1773(5) 0.164(5) Uani 1 1 d . A . H6A H 1.9637 -1.0581 0.1646 0.247 Uiso 1 1 calc R . . H6B H 1.8088 -1.0373 0.1443 0.247 Uiso 1 1 calc R . . H6C H 1.8599 -1.1325 0.1908 0.247 Uiso 1 1 calc R . . O5 O 1.4669(17) -0.943(2) 0.2986(15) 0.108(11) Uani 0.50 1 d PD A 3 C7 C 1.404(3) -1.0324(16) 0.2824(13) 0.116(11) Uani 0.50 1 d PD A 3 H7A H 1.4015 -1.0288 0.2390 0.140 Uiso 0.50 1 calc PR A 3 H7B H 1.4678 -1.0987 0.2934 0.140 Uiso 0.50 1 calc PR A 3 C8 C 1.268(3) -1.0440(19) 0.306(2) 0.143(12) Uani 0.50 1 d P A 3 H8A H 1.2656 -1.1196 0.3133 0.215 Uiso 0.50 1 calc PR A 3 H8B H 1.2000 -1.0138 0.2769 0.215 Uiso 0.50 1 calc PR A 3 H8C H 1.2468 -1.0066 0.3423 0.215 Uiso 0.50 1 calc PR A 3 O5' O 1.4788(15) -0.9669(18) 0.3072(13) 0.066(5) Uani 0.50 1 d PD A 4 C7' C 1.476(2) -1.0766(12) 0.2923(13) 0.088(6) Uani 0.50 1 d PD A 4 H7'A H 1.5510 -1.1280 0.3104 0.105 Uiso 0.50 1 calc PR A 4 H7'B H 1.4818 -1.0844 0.2492 0.105 Uiso 0.50 1 calc PR A 4 C8' C 1.338(3) -1.0889(19) 0.3188(17) 0.140(14) Uani 0.50 1 d P A 4 H8'A H 1.3122 -1.1523 0.3040 0.210 Uiso 0.50 1 calc PR A 4 H8'B H 1.2698 -1.0261 0.3080 0.210 Uiso 0.50 1 calc PR A 4 H8'C H 1.3421 -1.0965 0.3617 0.210 Uiso 0.50 1 calc PR A 4 O6 O 1.7371(14) -1.0233(10) 0.3382(4) 0.078(4) Uani 0.50 1 d PD A 5 C9 C 1.667(2) -1.0970(14) 0.3750(9) 0.165(10) Uani 0.50 1 d PD A 5 H9A H 1.5912 -1.1069 0.3505 0.198 Uiso 0.50 1 calc PR A 5 H9B H 1.7334 -1.1649 0.3738 0.198 Uiso 0.50 1 calc PR A 5 C10 C 1.608(3) -1.099(2) 0.4316(8) 0.205(18) Uani 0.50 1 d PD A 5 H10D H 1.5266 -1.1324 0.4320 0.308 Uiso 0.50 1 calc PR A 5 H10E H 1.5813 -1.0267 0.4449 0.308 Uiso 0.50 1 calc PR A 5 H10F H 1.6750 -1.1407 0.4579 0.308 Uiso 0.50 1 calc PR A 5 O6' O 1.6768(18) -0.9978(11) 0.3588(4) 0.108(6) Uani 0.50 1 d PD A 6 C9' C 1.7526(16) -1.0268(11) 0.4041(5) 0.071(4) Uani 0.50 1 d PD A 6 H9'A H 1.7963 -0.9694 0.4172 0.086 Uiso 0.50 1 calc PR A 6 H9'B H 1.8222 -1.0920 0.3979 0.086 Uiso 0.50 1 calc PR A 6 C10' C 1.640(2) -1.0446(16) 0.4408(9) 0.128(10) Uani 0.50 1 d PD A 6 H10A H 1.6507 -1.0231 0.4806 0.191 Uiso 0.50 1 calc PR A 6 H10B H 1.6348 -1.1203 0.4421 0.191 Uiso 0.50 1 calc PR A 6 H10C H 1.5549 -1.0030 0.4254 0.191 Uiso 0.50 1 calc PR A 6 C11 C 1.4401(5) -0.5482(4) 0.2907(2) 0.0467(13) Uani 1 1 d . A . H11A H 1.4375 -0.5200 0.2494 0.056 Uiso 1 1 calc R . . H11B H 1.3775 -0.4985 0.3163 0.056 Uiso 1 1 calc R . . C12 C 1.7174(5) -0.5007(4) 0.26978(19) 0.0446(13) Uani 1 1 d . . . C13 C 1.6604(6) -0.3994(4) 0.2497(2) 0.0515(14) Uani 1 1 d . . . H13A H 1.5663 -0.3716 0.2593 0.062 Uiso 1 1 calc R . . C14 C 1.7400(6) -0.3368(4) 0.2154(2) 0.0571(15) Uani 1 1 d . . . H14A H 1.6997 -0.2676 0.2011 0.068 Uiso 1 1 calc R . . C15 C 1.8768(6) -0.3767(5) 0.2025(2) 0.0592(15) Uani 1 1 d . . . H15A H 1.9312 -0.3345 0.1796 0.071 Uiso 1 1 calc R . . C16 C 1.9355(6) -0.4774(5) 0.2227(2) 0.0555(14) Uani 1 1 d . . . H16A H 2.0303 -0.5038 0.2140 0.067 Uiso 1 1 calc R . . C17 C 1.8562(6) -0.5408(4) 0.2557(2) 0.0516(14) Uani 1 1 d . . . H17A H 1.8964 -0.6109 0.2685 0.062 Uiso 1 1 calc R . . C18 C 1.6122(5) -0.5170(4) 0.3861(2) 0.0429(12) Uani 1 1 d . . . C19 C 1.7064(5) -0.5611(4) 0.4267(2) 0.0492(13) Uani 1 1 d . . . H19A H 1.7661 -0.6268 0.4197 0.059 Uiso 1 1 calc R . . C20 C 1.7142(6) -0.5085(5) 0.4787(2) 0.0592(16) Uani 1 1 d . . . H20A H 1.7793 -0.5386 0.5067 0.071 Uiso 1 1 calc R . . C21 C 1.6274(6) -0.4135(5) 0.4888(2) 0.0602(16) Uani 1 1 d . . . H21A H 1.6326 -0.3783 0.5239 0.072 Uiso 1 1 calc R . . C22 C 1.5332(6) -0.3693(5) 0.4484(2) 0.0592(15) Uani 1 1 d . . . H22A H 1.4731 -0.3039 0.4557 0.071 Uiso 1 1 calc R . . C23 C 1.5259(6) -0.4202(5) 0.3967(2) 0.0530(14) Uani 1 1 d . . . H23A H 1.4618 -0.3889 0.3685 0.064 Uiso 1 1 calc R . . C24 C 1.3082(6) -0.7022(4) 0.2353(2) 0.0509(14) Uani 1 1 d . A . C25 C 1.2186(8) -0.7719(5) 0.2394(2) 0.086(2) Uani 1 1 d . . . H25A H 1.2042 -0.8079 0.2762 0.103 Uiso 1 1 calc R A . C26 C 1.1489(7) -0.7912(6) 0.1918(3) 0.088(2) Uani 1 1 d . A . H26A H 1.0875 -0.8401 0.1959 0.105 Uiso 1 1 calc R . . C27 C 1.1681(6) -0.7402(5) 0.1390(2) 0.0646(16) Uani 1 1 d . . . H27A H 1.1218 -0.7545 0.1059 0.078 Uiso 1 1 calc R A . C28 C 1.2539(5) -0.6683(4) 0.1337(2) 0.0531(14) Uani 1 1 d . A . H28A H 1.2652 -0.6307 0.0972 0.064 Uiso 1 1 calc R . . C29 C 1.3255(5) -0.6499(4) 0.1823(2) 0.0459(12) Uani 1 1 d . . . H29A H 1.3865 -0.6007 0.1784 0.055 Uiso 1 1 calc R A . C30 C 1.2760(6) -0.6835(4) 0.3587(2) 0.0499(14) Uani 1 1 d . A . C31 C 1.1734(6) -0.5963(5) 0.3687(2) 0.0592(15) Uani 1 1 d . . . H31A H 1.1706 -0.5344 0.3436 0.071 Uiso 1 1 calc R A . C32 C 1.0742(6) -0.5965(5) 0.4145(3) 0.0672(17) Uani 1 1 d . A . H32A H 1.0056 -0.5351 0.4209 0.081 Uiso 1 1 calc R . . C33 C 1.0760(7) -0.6863(6) 0.4505(3) 0.0689(18) Uani 1 1 d . . . H33A H 1.0091 -0.6870 0.4821 0.083 Uiso 1 1 calc R A . C34 C 1.1745(7) -0.7748(6) 0.4407(2) 0.0699(18) Uani 1 1 d . A . H34A H 1.1735 -0.8371 0.4651 0.084 Uiso 1 1 calc R . . C35 C 1.2765(6) -0.7755(5) 0.3956(2) 0.0598(15) Uani 1 1 d . . . H35A H 1.3452 -0.8370 0.3899 0.072 Uiso 1 1 calc R A . C36 C 1.9502(6) -0.6439(5) -0.0120(2) 0.0665(17) Uani 1 1 d . . . H36A H 1.9678 -0.5856 -0.0392 0.100 Uiso 1 1 calc R . . H36B H 1.9305 -0.7019 -0.0343 0.100 Uiso 1 1 calc R . . H36C H 2.0314 -0.6697 0.0109 0.100 Uiso 1 1 calc R . . C37 C 1.8304(6) -0.6053(4) 0.0284(2) 0.0475(13) Uani 1 1 d . . . C38 C 1.8362(6) -0.5675(4) 0.0862(2) 0.0510(14) Uani 1 1 d . . . H38A H 1.9214 -0.5634 0.1067 0.061 Uiso 1 1 calc R . . C39 C 1.6996(6) -0.5326(4) 0.1075(2) 0.0519(14) Uani 1 1 d . . . H39A H 1.6725 -0.5013 0.1466 0.062 Uiso 1 1 calc R . . C40 C 1.6076(6) -0.5498(4) 0.0667(2) 0.0506(13) Uani 1 1 d . . . H40A H 1.5050 -0.5298 0.0701 0.061 Uiso 1 1 calc R . . C41 C 1.6900(6) -0.5949(4) 0.0169(2) 0.0507(13) Uani 1 1 d . . . H41A H 1.6536 -0.6123 -0.0206 0.061 Uiso 1 1 calc R . . N3 N 1.5067(5) -0.8143(3) 0.05459(18) 0.0492(11) Uani 1 1 d . . . C42 C 1.5897(5) -0.7712(4) 0.0704(2) 0.0448(12) Uani 1 1 d . . . C43 C 1.4069(5) -0.8696(4) 0.0382(2) 0.0473(13) Uani 1 1 d . . . C44 C 1.3324(6) -0.8288(5) -0.0095(2) 0.0570(15) Uani 1 1 d . . . C45 C 1.3558(7) -0.7295(6) -0.0436(3) 0.087(2) Uani 1 1 d . . . H45A H 1.3478 -0.6714 -0.0168 0.130 Uiso 1 1 calc R . . H45B H 1.2868 -0.7104 -0.0734 0.130 Uiso 1 1 calc R . . H45C H 1.4480 -0.7420 -0.0630 0.130 Uiso 1 1 calc R . . C46 C 1.2317(6) -0.8861(6) -0.0248(3) 0.0756(19) Uani 1 1 d . . . H46A H 1.1770 -0.8620 -0.0574 0.091 Uiso 1 1 calc R . . C47 C 1.2127(7) -0.9761(6) 0.0072(4) 0.077(2) Uani 1 1 d . . . H47A H 1.1455 -1.0142 -0.0038 0.092 Uiso 1 1 calc R . . C48 C 1.2885(7) -1.0120(5) 0.0546(4) 0.076(2) Uani 1 1 d . . . H48A H 1.2725 -1.0744 0.0762 0.092 Uiso 1 1 calc R . . C49 C 1.3888(6) -0.9593(4) 0.0722(3) 0.0554(15) Uani 1 1 d . . . C50 C 1.4702(7) -0.9959(5) 0.1247(3) 0.084(2) Uani 1 1 d . . . H50A H 1.5683 -1.0116 0.1128 0.126 Uiso 1 1 calc R . . H50B H 1.4421 -1.0602 0.1427 0.126 Uiso 1 1 calc R . . H50C H 1.4538 -0.9400 0.1533 0.126 Uiso 1 1 calc R . . P4 P 1.28198(18) -0.30852(14) 0.16576(7) 0.0694(5) Uani 1 1 d . . . F1 F 1.2533(6) -0.3529(4) 0.22924(19) 0.160(3) Uani 1 1 d . . . F2 F 1.1951(5) -0.3875(4) 0.1406(2) 0.1341(18) Uani 1 1 d . . . F3 F 1.3113(4) -0.2686(3) 0.09983(15) 0.0961(12) Uani 1 1 d . . . F4 F 1.1514(5) -0.2210(4) 0.1720(3) 0.172(3) Uani 1 1 d . . . F5 F 1.3738(6) -0.2335(3) 0.1865(2) 0.1343(18) Uani 1 1 d . . . F6 F 1.4128(4) -0.4004(3) 0.16005(15) 0.0780(10) Uani 1 1 d . . . Cl1 Cl 1.8693(3) -1.32462(19) 0.36864(10) 0.1308(9) Uani 1 1 d . . . Cl2 Cl 2.1481(3) -1.2959(2) 0.38127(11) 0.1320(9) Uani 1 1 d . . . C99 C 2.0054(10) -1.2744(7) 0.3354(4) 0.128(3) Uani 1 1 d . . . H99A H 1.9763 -1.1973 0.3266 0.153 Uiso 1 1 calc R . . H99B H 2.0334 -1.3090 0.2977 0.153 Uiso 1 1 calc R . . Cl4 Cl 1.8565(7) -0.9084(5) 0.5244(2) 0.153(2) Uani 0.50 1 d PD . . Cl3 Cl 2.0278(7) -1.0476(5) 0.4470(3) 0.165(2) Uani 0.50 1 d PD . . C98 C 1.9098(16) -0.9390(10) 0.4578(8) 0.121(7) Uani 0.50 1 d PD . . H98A H 1.9467 -0.8780 0.4391 0.145 Uiso 0.50 1 calc PR . . H98B H 1.8283 -0.9456 0.4362 0.145 Uiso 0.50 1 calc PR . . 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 0.0488(5) 0.0463(5) 0.0299(4) -0.0064(3) 0.0054(3) -0.0201(4) Mn2 0.0756(6) 0.0510(5) 0.0320(4) -0.0065(3) 0.0100(4) -0.0285(4) C1 0.060(4) 0.042(3) 0.040(3) -0.012(2) 0.007(2) -0.023(3) N1 0.070(3) 0.045(3) 0.035(2) -0.0088(19) 0.011(2) -0.025(2) N2 0.045(3) 0.052(3) 0.045(2) -0.012(2) -0.001(2) -0.017(2) O1 0.064(3) 0.063(3) 0.091(3) -0.025(2) -0.012(2) -0.004(2) C2 0.090(5) 0.056(4) 0.045(3) -0.003(3) 0.015(3) -0.029(4) O2 0.075(3) 0.091(3) 0.074(3) -0.007(2) 0.003(3) -0.021(3) C3 0.060(4) 0.047(3) 0.045(3) -0.003(2) 0.002(3) -0.018(3) O3 0.082(3) 0.064(2) 0.035(2) 0.0023(18) 0.0079(19) -0.013(2) P1 0.0540(9) 0.0514(8) 0.0307(6) -0.0089(6) 0.0046(6) -0.0264(7) P3 0.1394(18) 0.0544(10) 0.0390(8) -0.0021(7) 0.0073(9) -0.0448(11) P2 0.0699(10) 0.0549(8) 0.0305(7) -0.0047(6) 0.0017(6) -0.0387(8) O4 0.108(4) 0.058(3) 0.065(3) -0.017(2) 0.001(3) -0.020(2) C5 0.129(7) 0.076(5) 0.092(5) -0.017(4) 0.025(5) -0.027(5) C6 0.116(8) 0.108(7) 0.272(14) -0.090(8) 0.037(8) -0.019(6) O5 0.174(19) 0.070(15) 0.10(2) -0.017(12) 0.040(12) -0.097(13) C7 0.15(3) 0.068(15) 0.14(2) -0.071(16) 0.096(19) -0.059(14) C8 0.12(3) 0.060(16) 0.26(3) -0.046(18) 0.03(2) -0.050(14) O5' 0.128(12) 0.034(8) 0.045(6) -0.005(7) 0.025(6) -0.049(6) C7' 0.114(18) 0.035(10) 0.122(14) -0.015(10) 0.019(14) -0.037(10) C8' 0.14(3) 0.09(2) 0.21(3) -0.068(19) 0.10(3) -0.069(17) O6 0.150(11) 0.063(7) 0.022(5) 0.005(5) 0.009(6) -0.031(6) C9 0.24(3) 0.074(13) 0.18(2) 0.007(14) -0.08(2) -0.011(15) C10 0.38(5) 0.25(3) 0.032(9) 0.035(15) -0.012(16) -0.18(3) O6' 0.222(17) 0.084(10) 0.034(7) 0.024(7) -0.007(8) -0.076(10) C9' 0.097(11) 0.067(9) 0.043(7) -0.004(6) 0.005(7) 0.002(8) C10' 0.16(2) 0.086(14) 0.125(19) -0.028(13) -0.039(16) 0.019(14) C11 0.059(3) 0.054(3) 0.035(3) -0.001(2) -0.002(2) -0.032(3) C12 0.055(3) 0.056(3) 0.032(3) -0.010(2) 0.006(2) -0.033(3) C13 0.062(4) 0.055(3) 0.043(3) -0.012(3) 0.007(3) -0.025(3) C14 0.068(4) 0.055(3) 0.054(3) -0.004(3) 0.007(3) -0.029(3) C15 0.072(4) 0.064(4) 0.051(3) -0.004(3) 0.014(3) -0.041(3) C16 0.052(3) 0.073(4) 0.048(3) -0.018(3) 0.011(3) -0.029(3) C17 0.065(4) 0.057(3) 0.040(3) -0.011(2) 0.005(3) -0.027(3) C18 0.043(3) 0.057(3) 0.036(3) -0.008(2) 0.005(2) -0.026(3) C19 0.050(3) 0.062(3) 0.041(3) -0.010(3) 0.007(3) -0.023(3) C20 0.054(4) 0.094(5) 0.039(3) -0.009(3) -0.003(3) -0.037(4) C21 0.066(4) 0.082(4) 0.044(3) -0.031(3) 0.018(3) -0.039(4) C22 0.063(4) 0.074(4) 0.048(3) -0.028(3) 0.008(3) -0.027(3) C23 0.050(3) 0.070(4) 0.044(3) -0.016(3) 0.005(2) -0.022(3) C24 0.066(4) 0.065(3) 0.036(3) -0.010(2) 0.001(2) -0.045(3) C25 0.133(6) 0.111(5) 0.039(3) -0.001(3) -0.006(3) -0.089(5) C26 0.106(6) 0.123(6) 0.061(4) -0.012(4) -0.010(4) -0.087(5) C27 0.058(4) 0.093(5) 0.049(3) -0.021(3) -0.006(3) -0.026(3) C28 0.052(3) 0.069(4) 0.039(3) -0.009(3) 0.002(2) -0.015(3) C29 0.048(3) 0.057(3) 0.038(3) -0.012(2) 0.003(2) -0.022(3) C30 0.061(4) 0.062(3) 0.037(3) -0.001(3) -0.005(2) -0.036(3) C31 0.064(4) 0.074(4) 0.049(3) -0.002(3) -0.008(3) -0.035(3) C32 0.056(4) 0.093(5) 0.061(4) -0.013(4) 0.004(3) -0.036(3) C33 0.063(4) 0.105(5) 0.047(3) -0.003(4) 0.001(3) -0.039(4) C34 0.073(4) 0.102(5) 0.045(3) 0.020(3) -0.007(3) -0.047(4) C35 0.071(4) 0.073(4) 0.043(3) 0.005(3) 0.001(3) -0.036(3) C36 0.068(4) 0.080(4) 0.053(3) -0.006(3) 0.022(3) -0.025(3) C37 0.063(4) 0.045(3) 0.038(3) -0.003(2) 0.009(3) -0.024(3) C38 0.059(4) 0.057(3) 0.044(3) -0.001(3) 0.004(3) -0.033(3) C39 0.073(4) 0.043(3) 0.041(3) -0.007(2) 0.013(3) -0.017(3) C40 0.054(3) 0.049(3) 0.049(3) -0.002(3) -0.003(3) -0.011(3) C41 0.065(4) 0.051(3) 0.039(3) 0.004(2) 0.001(3) -0.019(3) N3 0.047(3) 0.050(3) 0.053(3) -0.020(2) 0.014(2) -0.016(2) C42 0.047(3) 0.050(3) 0.038(3) -0.009(2) 0.013(2) -0.012(3) C43 0.044(3) 0.053(3) 0.049(3) -0.025(3) 0.017(3) -0.020(3) C44 0.056(4) 0.071(4) 0.048(3) -0.025(3) 0.016(3) -0.021(3) C45 0.101(6) 0.113(6) 0.051(4) 0.002(4) -0.001(4) -0.036(5) C46 0.060(4) 0.108(6) 0.064(4) -0.052(4) 0.009(3) -0.018(4) C47 0.058(4) 0.079(5) 0.104(6) -0.053(4) 0.022(4) -0.036(4) C48 0.064(4) 0.054(4) 0.113(6) -0.030(4) 0.040(4) -0.022(3) C49 0.047(3) 0.047(3) 0.073(4) -0.021(3) 0.017(3) -0.013(3) C50 0.073(5) 0.069(4) 0.104(6) 0.002(4) 0.003(4) -0.004(4) P4 0.0708(12) 0.0666(11) 0.0641(10) 0.0097(9) 0.0163(9) -0.0053(10) F1 0.193(5) 0.148(4) 0.085(3) 0.048(3) 0.077(3) 0.062(4) F2 0.110(4) 0.135(4) 0.173(5) 0.041(3) -0.027(3) -0.070(3) F3 0.142(4) 0.086(3) 0.062(2) 0.0102(19) 0.001(2) -0.033(3) F4 0.129(4) 0.128(4) 0.211(6) 0.053(4) 0.052(4) 0.061(3) F5 0.197(5) 0.089(3) 0.128(4) -0.040(3) -0.039(4) -0.036(3) F6 0.075(2) 0.064(2) 0.089(2) -0.0118(18) 0.0186(19) -0.0046(18) Cl1 0.178(2) 0.1258(19) 0.1087(17) -0.0053(14) 0.0022(16) -0.0828(18) Cl2 0.161(2) 0.1324(19) 0.1194(18) -0.0297(15) 0.0290(17) -0.0749(18) C99 0.167(9) 0.131(7) 0.080(5) 0.003(5) 0.012(6) -0.024(7) Cl4 0.200(6) 0.142(5) 0.108(4) -0.027(3) -0.055(4) 0.013(4) Cl3 0.153(5) 0.158(5) 0.174(6) -0.011(4) 0.033(5) -0.019(4) C98 0.101(13) 0.058(9) 0.21(2) -0.030(11) 0.008(13) -0.031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N2 1.653(5) . ? Mn1 C42 1.892(6) . ? Mn1 C1 1.951(5) . ? Mn1 C41 2.114(5) . ? Mn1 C40 2.135(5) . ? Mn1 C37 2.151(5) . ? Mn1 C38 2.159(5) . ? Mn1 C39 2.160(5) . ? Mn2 C3 1.777(5) . ? Mn2 C2 1.806(8) . ? Mn2 N1 2.012(4) . ? Mn2 P3 2.2239(17) . ? Mn2 P1 2.2977(15) . ? Mn2 P2 2.3581(18) . ? C1 N1 1.157(5) . ? N2 O1 1.182(5) . ? C2 O2 1.159(7) . ? C3 O3 1.162(5) . ? P1 C18 1.815(5) . ? P1 C12 1.826(5) . ? P1 C11 1.837(5) . ? P3 O6' 1.579(10) . ? P3 O4 1.595(4) . ? P3 O5' 1.597(11) . ? P3 O5 1.607(13) . ? P3 O6 1.689(11) . ? P2 C30 1.814(5) . ? P2 C24 1.828(5) . ? P2 C11 1.839(5) . ? O4 C5 1.439(8) . ? C5 C6 1.400(10) . ? O5 C7 1.478(14) . ? C7 C8 1.45(4) . ? O5' C7' 1.472(14) . ? C7' C8' 1.49(4) . ? O6 C9 1.476(18) . ? C9 C10 1.383(18) . ? O6' C9' 1.309(18) . ? C9' C10' 1.402(18) . ? C12 C13 1.381(7) . ? C12 C17 1.400(7) . ? C13 C14 1.406(7) . ? C14 C15 1.375(8) . ? C15 C16 1.380(8) . ? C16 C17 1.395(7) . ? C18 C19 1.375(7) . ? C18 C23 1.393(7) . ? C19 C20 1.408(7) . ? C20 C21 1.375(8) . ? C21 C22 1.373(8) . ? C22 C23 1.390(7) . ? C24 C29 1.366(6) . ? C24 C25 1.369(7) . ? C25 C26 1.379(8) . ? C26 C27 1.359(8) . ? C27 C28 1.364(7) . ? C28 C29 1.405(7) . ? C30 C31 1.381(8) . ? C30 C35 1.411(7) . ? C31 C32 1.391(7) . ? C32 C33 1.375(8) . ? C33 C34 1.370(8) . ? C34 C35 1.397(8) . ? C36 C37 1.483(7) . ? C37 C41 1.411(7) . ? C37 C38 1.439(7) . ? C38 C39 1.409(7) . ? C39 C40 1.395(7) . ? C40 C41 1.440(7) . ? N3 C42 1.158(6) . ? N3 C43 1.399(6) . ? C43 C44 1.375(8) . ? C43 C49 1.386(7) . ? C44 C46 1.415(8) . ? C44 C45 1.504(8) . ? C46 C47 1.368(9) . ? C47 C48 1.362(9) . ? C48 C49 1.391(8) . ? C49 C50 1.489(8) . ? P4 F4 1.550(5) . ? P4 F5 1.552(5) . ? P4 F1 1.556(4) . ? P4 F6 1.584(4) . ? P4 F3 1.589(4) . ? P4 F2 1.596(5) . ? Cl1 C99 1.721(9) . ? Cl2 C99 1.779(9) . ? Cl4 Cl3 1.364(8) 2_936 ? Cl4 C98 1.622(14) . ? Cl3 Cl4 1.364(8) 2_936 ? Cl3 C98 1.662(12) . ? 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 N2 Mn1 C42 96.2(2) . . ? N2 Mn1 C1 96.2(2) . . ? C42 Mn1 C1 91.5(2) . . ? N2 Mn1 C41 119.0(2) . . ? C42 Mn1 C41 89.6(2) . . ? C1 Mn1 C41 144.4(2) . . ? N2 Mn1 C40 157.6(2) . . ? C42 Mn1 C40 90.9(2) . . ? C1 Mn1 C40 104.8(2) . . ? C41 Mn1 C40 39.62(19) . . ? N2 Mn1 C37 92.8(2) . . ? C42 Mn1 C37 122.3(2) . . ? C1 Mn1 C37 143.73(19) . . ? C41 Mn1 C37 38.63(19) . . ? C40 Mn1 C37 65.6(2) . . ? N2 Mn1 C38 102.7(2) . . ? C42 Mn1 C38 153.4(2) . . ? C1 Mn1 C38 104.74(19) . . ? C41 Mn1 C38 64.8(2) . . ? C40 Mn1 C38 64.8(2) . . ? C37 Mn1 C38 39.01(18) . . ? N2 Mn1 C39 138.7(2) . . ? C42 Mn1 C39 124.9(2) . . ? C1 Mn1 C39 86.56(19) . . ? C41 Mn1 C39 64.2(2) . . ? C40 Mn1 C39 37.89(19) . . ? C37 Mn1 C39 64.27(19) . . ? C38 Mn1 C39 38.07(19) . . ? C3 Mn2 C2 89.8(2) . . ? C3 Mn2 N1 176.3(2) . . ? C2 Mn2 N1 93.3(2) . . ? C3 Mn2 P3 90.64(17) . . ? C2 Mn2 P3 91.37(19) . . ? N1 Mn2 P3 91.20(12) . . ? C3 Mn2 P1 92.03(16) . . ? C2 Mn2 P1 97.38(19) . . ? N1 Mn2 P1 85.67(12) . . ? P3 Mn2 P1 170.85(8) . . ? C3 Mn2 P2 91.79(18) . . ? C2 Mn2 P2 169.56(19) . . ? N1 Mn2 P2 84.81(13) . . ? P3 Mn2 P2 98.92(7) . . ? P1 Mn2 P2 72.26(5) . . ? N1 C1 Mn1 177.0(5) . . ? C1 N1 Mn2 176.3(4) . . ? O1 N2 Mn1 176.5(4) . . ? O2 C2 Mn2 177.8(5) . . ? O3 C3 Mn2 178.8(5) . . ? C18 P1 C12 100.7(2) . . ? C18 P1 C11 106.8(2) . . ? C12 P1 C11 106.3(2) . . ? C18 P1 Mn2 121.62(17) . . ? C12 P1 Mn2 123.91(18) . . ? C11 P1 Mn2 95.46(16) . . ? O6' P3 O4 112.6(6) . . ? O6' P3 O5' 93.1(13) . . ? O4 P3 O5' 99.1(9) . . ? O6' P3 O5 104.9(13) . . ? O4 P3 O5 98.8(12) . . ? O4 P3 O6 87.4(4) . . ? O5' P3 O6 107.6(11) . . ? O5 P3 O6 120.4(12) . . ? O6' P3 Mn2 109.2(5) . . ? O4 P3 Mn2 119.63(17) . . ? O5' P3 Mn2 120.1(8) . . ? O5 P3 Mn2 110.3(10) . . ? O6 P3 Mn2 117.3(5) . . ? C30 P2 C24 102.1(2) . . ? C30 P2 C11 106.1(2) . . ? C24 P2 C11 106.7(2) . . ? C30 P2 Mn2 120.70(19) . . ? C24 P2 Mn2 125.15(19) . . ? C11 P2 Mn2 93.39(17) . . ? C5 O4 P3 121.0(4) . . ? C6 C5 O4 112.7(7) . . ? C7 O5 P3 132(2) . . ? C8 C7 O5 121(2) . . ? C7' O5' P3 117.2(17) . . ? O5' C7' C8' 100.5(17) . . ? C9 O6 P3 111.9(11) . . ? C10 C9 O6 136.1(19) . . ? C9' O6' P3 157.4(14) . . ? O6' C9' C10' 93.0(16) . . ? P1 C11 P2 96.6(2) . . ? C13 C12 C17 119.2(4) . . ? C13 C12 P1 120.8(4) . . ? C17 C12 P1 120.0(4) . . ? C12 C13 C14 120.8(5) . . ? C15 C14 C13 119.4(5) . . ? C14 C15 C16 120.5(5) . . ? C15 C16 C17 120.3(5) . . ? C16 C17 C12 119.7(5) . . ? C19 C18 C23 119.6(5) . . ? C19 C18 P1 118.7(4) . . ? C23 C18 P1 121.5(4) . . ? C18 C19 C20 119.8(5) . . ? C21 C20 C19 120.0(5) . . ? C22 C21 C20 120.4(5) . . ? C21 C22 C23 120.0(6) . . ? C22 C23 C18 120.3(5) . . ? C29 C24 C25 118.1(5) . . ? C29 C24 P2 121.7(4) . . ? C25 C24 P2 120.2(4) . . ? C24 C25 C26 121.8(5) . . ? C27 C26 C25 119.9(6) . . ? C26 C27 C28 119.8(5) . . ? C27 C28 C29 119.9(5) . . ? C24 C29 C28 120.5(5) . . ? C31 C30 C35 118.2(5) . . ? C31 C30 P2 122.1(4) . . ? C35 C30 P2 119.7(5) . . ? C30 C31 C32 121.9(6) . . ? C33 C32 C31 119.5(6) . . ? C34 C33 C32 119.8(6) . . ? C33 C34 C35 121.5(6) . . ? C34 C35 C30 119.0(6) . . ? C41 C37 C38 107.0(5) . . ? C41 C37 C36 127.0(5) . . ? C38 C37 C36 126.0(5) . . ? C41 C37 Mn1 69.3(3) . . ? C38 C37 Mn1 70.8(3) . . ? C36 C37 Mn1 126.7(4) . . ? C39 C38 C37 107.2(5) . . ? C39 C38 Mn1 71.0(3) . . ? C37 C38 Mn1 70.2(3) . . ? C40 C39 C38 110.3(5) . . ? C40 C39 Mn1 70.1(3) . . ? C38 C39 Mn1 70.9(3) . . ? C39 C40 C41 106.4(5) . . ? C39 C40 Mn1 72.0(3) . . ? C41 C40 Mn1 69.4(3) . . ? C37 C41 C40 109.0(5) . . ? C37 C41 Mn1 72.1(3) . . ? C40 C41 Mn1 71.0(3) . . ? C42 N3 C43 177.0(5) . . ? N3 C42 Mn1 176.3(4) . . ? C44 C43 C49 125.3(5) . . ? C44 C43 N3 117.2(5) . . ? C49 C43 N3 117.5(5) . . ? C43 C44 C46 115.8(6) . . ? C43 C44 C45 122.4(5) . . ? C46 C44 C45 121.8(6) . . ? C47 C46 C44 120.4(6) . . ? C48 C47 C46 121.2(6) . . ? C47 C48 C49 121.5(6) . . ? C43 C49 C48 115.9(6) . . ? C43 C49 C50 122.0(5) . . ? C48 C49 C50 122.2(6) . . ? F4 P4 F5 91.5(3) . . ? F4 P4 F1 90.4(3) . . ? F5 P4 F1 93.3(3) . . ? F4 P4 F6 178.4(3) . . ? F5 P4 F6 89.8(2) . . ? F1 P4 F6 88.6(2) . . ? F4 P4 F3 91.1(3) . . ? F5 P4 F3 88.9(2) . . ? F1 P4 F3 177.3(3) . . ? F6 P4 F3 89.9(2) . . ? F4 P4 F2 91.1(3) . . ? F5 P4 F2 176.0(3) . . ? F1 P4 F2 89.7(3) . . ? F6 P4 F2 87.7(2) . . ? F3 P4 F2 88.0(2) . . ? Cl1 C99 Cl2 111.2(4) . . ? Cl3 Cl4 C98 99.1(8) 2_936 . ? Cl4 Cl3 C98 132.4(8) 2_936 . ? Cl4 C98 Cl3 119.4(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.511 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.068 #===END data_cis-9[PF6].CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 644603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H63 Cl2 F6 Mn2 N3 O6 P4' _chemical_formula_weight 1364.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.651(2) _cell_length_b 14.574(3) _cell_length_c 18.143(3) _cell_angle_alpha 68.629(3) _cell_angle_beta 79.220(3) _cell_angle_gamma 71.517(3) _cell_volume 3177.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 74 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.778260 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27758 _diffrn_reflns_av_R_equivalents 0.1009 _diffrn_reflns_av_sigmaI/netI 0.1650 _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 -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11185 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+5.5535P] 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 11185 _refine_ls_number_parameters 922 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2068 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2493 _refine_ls_wR_factor_gt 0.1866 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.03375(9) -0.26689(13) -0.74232(9) 0.0730(5) Uani 1 1 d . . . Mn2 Mn 1.41174(8) -0.30620(9) -0.71963(7) 0.0421(4) Uani 1 1 d . A . C1 C 1.1747(7) -0.2760(6) -0.7296(5) 0.055(2) Uani 1 1 d . . . N1 N 1.2609(5) -0.2847(5) -0.7242(4) 0.0490(17) Uani 1 1 d . . . N2 N 1.0292(6) -0.2032(10) -0.8369(5) 0.120(4) Uani 1 1 d . . . O1 O 1.0174(6) -0.1592(12) -0.9049(6) 0.214(7) Uani 1 1 d . . . C2 C 1.4232(6) -0.4339(6) -0.6524(5) 0.046(2) Uani 1 1 d . . . O2 O 1.4316(5) -0.5135(5) -0.6048(4) 0.0736(19) Uani 1 1 d . . . C3 C 1.5444(7) -0.3275(8) -0.7179(8) 0.095(4) Uani 1 1 d . . . O3 O 1.6332(5) -0.3472(7) -0.7138(9) 0.210(7) Uani 1 1 d . . . P1 P 1.36259(16) -0.23176(16) -0.62141(12) 0.0473(6) Uani 1 1 d . A . P2 P 1.37412(15) -0.12720(16) -0.77800(12) 0.0424(5) Uani 1 1 d . . . P3 P 1.4451(2) -0.34460(18) -0.83004(15) 0.0730(8) Uani 1 1 d . . . O4 O 1.4991(6) -0.4493(5) -0.8367(4) 0.103(3) Uani 1 1 d . A . O5 O 1.4803(9) -0.2684(11) -0.9085(9) 0.071(4) Uani 0.634(6) 1 d P A 1 O6 O 1.3286(6) -0.3488(7) -0.8610(5) 0.058(3) Uani 0.634(6) 1 d P A 1 C4 C 1.5182(9) -0.5454(7) -0.7766(5) 0.066(3) Uani 1 1 d . . . C5 C 1.6102(8) -0.5804(8) -0.7417(6) 0.073(3) Uani 1 1 d . A . H5A H 1.6572 -0.5394 -0.7564 0.087 Uiso 1 1 calc R . . C6 C 1.6327(7) -0.6769(7) -0.6843(6) 0.072(3) Uani 1 1 d . . . H6A H 1.6951 -0.7018 -0.6587 0.087 Uiso 1 1 calc R A . C7 C 1.5656(8) -0.7360(7) -0.6647(6) 0.074(3) Uani 1 1 d . A . H7A H 1.5820 -0.8026 -0.6266 0.088 Uiso 1 1 calc R . . C8 C 1.4746(8) -0.6988(8) -0.7003(6) 0.069(3) Uani 1 1 d . . . H8A H 1.4270 -0.7392 -0.6855 0.083 Uiso 1 1 calc R A . C9 C 1.4509(8) -0.6024(8) -0.7578(5) 0.066(3) Uani 1 1 d . A . H9A H 1.3884 -0.5773 -0.7833 0.079 Uiso 1 1 calc R . . C10 C 1.5572(10) -0.2908(10) -0.9695(9) 0.059(4) Uani 0.634(6) 1 d P A 1 C11 C 1.652(2) -0.328(2) -0.9477(19) 0.088(9) Uani 0.634(6) 1 d P A 1 H11A H 1.6674 -0.3367 -0.8960 0.105 Uiso 0.634(6) 1 calc PR A 1 C12 C 1.7322(14) -0.353(2) -1.0063(13) 0.123(10) Uani 0.634(6) 1 d P A 1 H12A H 1.7992 -0.3929 -0.9897 0.147 Uiso 0.634(6) 1 calc PR A 1 C13 C 1.718(3) -0.326(2) -1.077(2) 0.14(2) Uani 0.634(6) 1 d P A 1 H13A H 1.7756 -0.3320 -1.1159 0.169 Uiso 0.634(6) 1 calc PR A 1 C14 C 1.6133(14) -0.2849(13) -1.1009(9) 0.081(5) Uani 0.634(6) 1 d P A 1 H14A H 1.5994 -0.2717 -1.1538 0.098 Uiso 0.634(6) 1 calc PR A 1 C15 C 1.5355(12) -0.2659(11) -1.0456(9) 0.070(4) Uani 0.634(6) 1 d P A 1 H15A H 1.4661 -0.2352 -1.0599 0.084 Uiso 0.634(6) 1 calc PR A 1 C16 C 1.3190(8) -0.3420(8) -0.9372(5) 0.057(4) Uani 0.634(6) 1 d PG A 1 C17 C 1.3642(7) -0.4250(7) -0.9644(6) 0.069(4) Uani 0.634(6) 1 d PG A 1 H17A H 1.4048 -0.4871 -0.9309 0.083 Uiso 0.634(6) 1 calc PR A 1 C18 C 1.3498(9) -0.4172(9) -1.0405(6) 0.074(5) Uani 0.634(6) 1 d PG A 1 H18A H 1.3807 -0.4739 -1.0591 0.089 Uiso 0.634(6) 1 calc PR A 1 C19 C 1.2904(10) -0.3264(11) -1.0895(5) 0.093(8) Uani 0.634(6) 1 d PG A 1 H19A H 1.2806 -0.3210 -1.1416 0.112 Uiso 0.634(6) 1 calc PR A 1 C20 C 1.2453(9) -0.2434(8) -1.0624(8) 0.099(10) Uani 0.634(6) 1 d PG A 1 H20A H 1.2046 -0.1813 -1.0959 0.118 Uiso 0.634(6) 1 calc PR A 1 C21 C 1.2596(9) -0.2512(7) -0.9863(8) 0.072(6) Uani 0.634(6) 1 d PG A 1 H21A H 1.2287 -0.1945 -0.9677 0.087 Uiso 0.634(6) 1 calc PR A 1 C22 C 1.4739(6) -0.0613(7) -0.7836(6) 0.034(5) Uani 0.50 1 d PG B 1 C23 C 1.5795(7) -0.1094(6) -0.7811(4) 0.059(5) Uani 0.50 1 d PG B 1 H23 H 1.6044 -0.1803 -0.7748 0.071 Uiso 0.50 1 calc PR B 1 C24 C 1.6486(7) -0.0538(8) -0.7879(8) 0.072(6) Uani 0.50 1 d PG B 1 H24 H 1.7208 -0.0866 -0.7863 0.086 Uiso 0.50 1 calc PR B 1 C25 C 1.6121(9) 0.0500(8) -0.7972(7) 0.086(9) Uani 0.50 1 d PG B 1 H25 H 1.6593 0.0880 -0.8018 0.104 Uiso 0.50 1 calc PR B 1 C26 C 1.5065(10) 0.0981(6) -0.7996(6) 0.087(7) Uani 0.50 1 d PG B 1 H26 H 1.4815 0.1690 -0.8059 0.104 Uiso 0.50 1 calc PR B 1 C27 C 1.4374(8) 0.0424(7) -0.7928(8) 0.061(5) Uani 0.50 1 d PG B 1 H27 H 1.3652 0.0753 -0.7945 0.073 Uiso 0.50 1 calc PR B 1 O5' O 1.5910(10) -0.3474(7) -0.8538(8) 0.047(4) Uani 0.366(6) 1 d PG A 2 C10' C 1.6436(18) -0.3493(12) -0.9281(9) 0.051(14) Uani 0.366(6) 1 d PG A 2 C11' C 1.6684(17) -0.2617(11) -0.9814(11) 0.064(9) Uani 0.366(6) 1 d PG A 2 H11B H 1.6579 -0.2039 -0.9653 0.077 Uiso 0.366(6) 1 calc PR A 2 C12' C 1.7088(19) -0.2587(14) -1.0582(10) 0.084(12) Uani 0.366(6) 1 d PG A 2 H12B H 1.7258 -0.1988 -1.0947 0.100 Uiso 0.366(6) 1 calc PR A 2 C13' C 1.724(2) -0.3433(18) -1.0818(9) 0.056(16) Uani 0.366(6) 1 d PG A 2 H13B H 1.7518 -0.3412 -1.1343 0.068 Uiso 0.366(6) 1 calc PR A 2 C14' C 1.6993(16) -0.4309(14) -1.0285(12) 0.092(11) Uani 0.366(6) 1 d PG A 2 H14B H 1.7099 -0.4887 -1.0446 0.111 Uiso 0.366(6) 1 calc PR A 2 C15' C 1.6590(16) -0.4339(10) -0.9517(11) 0.074(9) Uani 0.366(6) 1 d PG A 2 H15B H 1.6420 -0.4937 -0.9153 0.089 Uiso 0.366(6) 1 calc PR A 2 O6' O 1.4216(16) -0.2664(14) -0.9059(11) 0.043(5) Uani 0.366(6) 1 d P A 2 C16' C 1.3674(12) -0.2782(13) -0.9585(7) 0.036(5) Uani 0.366(6) 1 d PG A 2 C17' C 1.4194(10) -0.3006(14) -1.0261(9) 0.064(8) Uani 0.366(6) 1 d PG A 2 H17B H 1.4926 -0.3141 -1.0341 0.077 Uiso 0.366(6) 1 calc PR A 2 C18' C 1.3640(14) -0.3033(16) -1.0819(8) 0.067(8) Uani 0.366(6) 1 d PG A 2 H18B H 1.3995 -0.3186 -1.1281 0.080 Uiso 0.366(6) 1 calc PR A 2 C19' C 1.2568(14) -0.2836(19) -1.0702(11) 0.060(11) Uani 0.366(6) 1 d PG A 2 H19B H 1.2190 -0.2854 -1.1084 0.072 Uiso 0.366(6) 1 calc PR A 2 C20' C 1.2049(10) -0.261(2) -1.0026(13) 0.130(19) Uani 0.366(6) 1 d PG A 2 H20B H 1.1316 -0.2477 -0.9946 0.156 Uiso 0.366(6) 1 calc PR A 2 C21' C 1.2602(12) -0.2585(17) -0.9468(10) 0.112(17) Uani 0.366(6) 1 d PG A 2 H21B H 1.2247 -0.2431 -0.9006 0.134 Uiso 0.366(6) 1 calc PR A 2 C28 C 1.2746(9) -0.0366(8) -0.8534(7) 0.041(6) Uani 0.50 1 d PG B 1 C29 C 1.2569(9) 0.0687(8) -0.8748(8) 0.059(5) Uani 0.50 1 d PG B 1 H29A H 1.2996 0.0957 -0.8572 0.071 Uiso 0.50 1 calc PR B 1 C30 C 1.1769(9) 0.1346(7) -0.9219(8) 0.084(7) Uani 0.50 1 d PG B 1 H30A H 1.1648 0.2066 -0.9365 0.100 Uiso 0.50 1 calc PR B 1 C31 C 1.1145(8) 0.0951(9) -0.9476(7) 0.058(5) Uani 0.50 1 d PG B 1 H31A H 1.0598 0.1401 -0.9798 0.069 Uiso 0.50 1 calc PR B 1 C32 C 1.1321(10) -0.0102(10) -0.9263(8) 0.080(8) Uani 0.50 1 d PG B 1 H32A H 1.0895 -0.0372 -0.9439 0.096 Uiso 0.50 1 calc PR B 1 C33 C 1.2122(11) -0.0761(7) -0.8792(8) 0.055(5) Uani 0.50 1 d PG B 1 H33A H 1.2242 -0.1481 -0.8646 0.066 Uiso 0.50 1 calc PR B 1 C22' C 1.4776(7) -0.0680(10) -0.8140(6) 0.037(5) Uani 0.50 1 d PG B 4 C23' C 1.5402(9) -0.0835(9) -0.8807(6) 0.061(5) Uani 0.50 1 d PG B 4 H23B H 1.5256 -0.1224 -0.9073 0.073 Uiso 0.50 1 calc PR B 4 C24' C 1.6241(8) -0.0421(10) -0.9083(6) 0.066(5) Uani 0.50 1 d PG B 4 H24B H 1.6669 -0.0526 -0.9538 0.080 Uiso 0.50 1 calc PR B 4 C25' C 1.6455(8) 0.0148(10) -0.8692(8) 0.081(6) Uani 0.50 1 d PG B 4 H25B H 1.7029 0.0431 -0.8881 0.097 Uiso 0.50 1 calc PR B 4 C26' C 1.5829(11) 0.0303(10) -0.8026(8) 0.070(7) Uani 0.50 1 d PG B 4 H26B H 1.5975 0.0691 -0.7759 0.084 Uiso 0.50 1 calc PR B 4 C27' C 1.4990(9) -0.0112(10) -0.7750(6) 0.061(6) Uani 0.50 1 d PG B 4 H27B H 1.4562 -0.0006 -0.7295 0.073 Uiso 0.50 1 calc PR B 4 C28' C 1.3123(12) -0.0575(10) -0.8636(6) 0.060(8) Uani 0.50 1 d PG B 2 C29' C 1.3728(9) -0.0451(11) -0.9354(8) 0.074(6) Uani 0.50 1 d PG B 2 H29' H 1.4460 -0.0722 -0.9358 0.088 Uiso 0.50 1 calc PR B 2 C30' C 1.3263(12) 0.0070(11) -1.0065(6) 0.088(7) Uani 0.50 1 d PG B 2 H30' H 1.3677 0.0155 -1.0556 0.106 Uiso 0.50 1 calc PR B 2 C31' C 1.2193(13) 0.0467(10) -1.0059(8) 0.099(8) Uani 0.50 1 d PG B 2 H31' H 1.1875 0.0822 -1.0545 0.118 Uiso 0.50 1 calc PR B 2 C32' C 1.1587(9) 0.0342(12) -0.9341(11) 0.080(8) Uani 0.50 1 d PG B 2 H32' H 1.0856 0.0614 -0.9337 0.096 Uiso 0.50 1 calc PR B 2 C33' C 1.2052(12) -0.0178(11) -0.8630(8) 0.067(6) Uani 0.50 1 d PG B 2 H33' H 1.1639 -0.0263 -0.8139 0.080 Uiso 0.50 1 calc PR B 2 C34 C 1.2720(6) -0.2723(7) -0.5383(5) 0.054(2) Uani 1 1 d . . . C35 C 1.1794(7) -0.2057(8) -0.5221(5) 0.070(3) Uani 1 1 d . B . H35A H 1.1630 -0.1359 -0.5546 0.085 Uiso 1 1 calc R . . C36 C 1.1095(8) -0.2401(10) -0.4583(7) 0.089(3) Uani 1 1 d . . . H36A H 1.0458 -0.1941 -0.4479 0.107 Uiso 1 1 calc R B . C37 C 1.1348(10) -0.3426(11) -0.4105(6) 0.093(4) Uani 1 1 d . B . H37A H 1.0877 -0.3670 -0.3675 0.112 Uiso 1 1 calc R . . C38 C 1.2281(10) -0.4088(9) -0.4254(6) 0.098(4) Uani 1 1 d . . . H38A H 1.2459 -0.4784 -0.3921 0.117 Uiso 1 1 calc R B . C39 C 1.2959(8) -0.3733(8) -0.4891(5) 0.080(3) Uani 1 1 d . B . H39A H 1.3599 -0.4192 -0.4991 0.096 Uiso 1 1 calc R . . C40 C 1.4603(8) -0.2112(8) -0.5783(5) 0.064(3) Uani 1 1 d . . . C41 C 1.4591(9) -0.1187(10) -0.5752(6) 0.096(4) Uani 1 1 d . B . H41A H 1.4030 -0.0603 -0.5944 0.115 Uiso 1 1 calc R . . C42' C 1.5401(14) -0.1100(17) -0.5441(10) 0.150(9) Uani 1 1 d . . . H42A H 1.5415 -0.0445 -0.5457 0.180 Uiso 1 1 calc R B . C42 C 0.9837(6) -0.1533(8) -0.7061(5) 0.063(3) Uani 1 1 d . . . N3 N 0.9484(6) -0.0821(7) -0.6865(5) 0.073(2) Uani 1 1 d . . . C43 C 1.6147(16) -0.191(2) -0.5125(8) 0.168(11) Uani 1 1 d . B . H43A H 1.6671 -0.1829 -0.4893 0.201 Uiso 1 1 calc R . . C44 C 1.6191(11) -0.2852(13) -0.5121(8) 0.160(8) Uani 1 1 d . . . H44A H 1.6732 -0.3433 -0.4885 0.192 Uiso 1 1 calc R B . C45 C 1.5423(10) -0.2947(10) -0.5471(7) 0.119(5) Uani 1 1 d . B . H45A H 1.5459 -0.3596 -0.5498 0.143 Uiso 1 1 calc R . . C46 C 0.9913(12) -0.3683(11) -0.6308(7) 0.111(5) Uani 1 1 d . . . C47 C 1.0718(9) -0.4282(9) -0.6683(7) 0.086(3) Uani 1 1 d . . . C48 C 1.0391(7) -0.4172(9) -0.7409(6) 0.083(3) Uani 1 1 d . . . C49 C 0.9370(7) -0.3530(10) -0.7476(9) 0.129(6) Uani 1 1 d . . . C50 C 0.9069(9) -0.3228(13) -0.6816(12) 0.162(8) Uani 1 1 d . . . C51 C 0.9928(16) -0.3591(13) -0.5512(8) 0.212(10) Uani 1 1 d . . . H51A H 0.9549 -0.4040 -0.5107 0.318 Uiso 1 1 calc R . . H51B H 0.9599 -0.2880 -0.5531 0.318 Uiso 1 1 calc R . . H51C H 1.0647 -0.3791 -0.5380 0.318 Uiso 1 1 calc R . . C52 C 1.1741(10) -0.4960(9) -0.6364(7) 0.118(5) Uani 1 1 d . . . H52A H 1.1694 -0.5665 -0.6106 0.177 Uiso 1 1 calc R . . H52B H 1.1908 -0.4719 -0.5976 0.177 Uiso 1 1 calc R . . H52C H 1.2285 -0.4936 -0.6801 0.177 Uiso 1 1 calc R . . C53 C 1.1021(7) -0.4698(8) -0.7996(6) 0.093(4) Uani 1 1 d . . . H53A H 1.1006 -0.5416 -0.7800 0.140 Uiso 1 1 calc R . . H53B H 1.1739 -0.4665 -0.8056 0.140 Uiso 1 1 calc R . . H53C H 1.0724 -0.4354 -0.8511 0.140 Uiso 1 1 calc R . . C54 C 0.8715(10) -0.3265(13) -0.8153(12) 0.219(11) Uani 1 1 d . . . H54A H 0.8268 -0.3726 -0.8001 0.328 Uiso 1 1 calc R . . H54B H 0.9168 -0.3343 -0.8627 0.328 Uiso 1 1 calc R . . H54C H 0.8285 -0.2556 -0.8270 0.328 Uiso 1 1 calc R . . C55 C 0.8017(10) -0.2594(19) -0.6603(19) 0.40(2) Uani 1 1 d . . . H55A H 0.7541 -0.3028 -0.6383 0.598 Uiso 1 1 calc R . . H55B H 0.7749 -0.2037 -0.7080 0.598 Uiso 1 1 calc R . . H55C H 0.8077 -0.2307 -0.6207 0.598 Uiso 1 1 calc R . . C56 C 0.8970(7) 0.0154(8) -0.6704(7) 0.073(3) Uani 1 1 d . . . C57 C 0.925(2) 0.0977(13) -0.7285(13) 0.309(19) Uani 1 1 d . . . H57A H 0.8922 0.1598 -0.7140 0.463 Uiso 1 1 calc R . . H57B H 0.9020 0.1069 -0.7794 0.463 Uiso 1 1 calc R . . H57C H 1.0005 0.0848 -0.7332 0.463 Uiso 1 1 calc R . . C58 C 0.920(2) 0.0048(13) -0.5940(12) 0.278(15) Uani 1 1 d . . . H58A H 0.8811 0.0669 -0.5809 0.416 Uiso 1 1 calc R . . H58B H 0.9941 -0.0055 -0.5938 0.416 Uiso 1 1 calc R . . H58C H 0.8992 -0.0543 -0.5545 0.416 Uiso 1 1 calc R . . C59 C 0.7893(11) 0.0264(18) -0.663(2) 0.40(3) Uani 1 1 d . . . H59A H 0.7531 0.0792 -0.6380 0.607 Uiso 1 1 calc R . . H59B H 0.7754 -0.0389 -0.6291 0.607 Uiso 1 1 calc R . . H59C H 0.7648 0.0465 -0.7151 0.607 Uiso 1 1 calc R . . C60 C 1.2983(6) -0.1066(6) -0.6885(4) 0.045(2) Uani 1 1 d . A . H60A H 1.2234 -0.0973 -0.6895 0.054 Uiso 1 1 calc R . . H60B H 1.3088 -0.0490 -0.6771 0.054 Uiso 1 1 calc R . . P4 P 1.1928(2) 0.1915(2) -0.65821(16) 0.0738(8) Uani 1 1 d . C 4 F1 F 1.0790(5) 0.2581(6) -0.6871(4) 0.128(2) Uani 1 1 d . C 4 F2 F 1.3038(4) 0.1255(4) -0.6299(4) 0.110(2) Uani 1 1 d . C 4 F3 F 1.1496(5) 0.0951(5) -0.6097(4) 0.118(2) Uani 1 1 d . C 4 F4 F 1.2173(7) 0.1543(6) -0.7334(4) 0.144(3) Uani 1 1 d . C 4 F5 F 1.2371(5) 0.2849(4) -0.7079(4) 0.111(2) Uani 1 1 d . C 4 F6 F 1.1668(4) 0.2278(5) -0.5845(3) 0.102(2) Uani 1 1 d . C 4 C99 C 2.0084(12) -0.3581(17) -1.1298(12) 0.212(10) Uani 1 1 d . D 4 H99A H 1.9605 -0.3994 -1.1241 0.255 Uiso 1 1 calc R D 4 H99B H 1.9754 -0.2868 -1.1616 0.255 Uiso 1 1 calc R D 4 Cl1 Cl 2.0209(4) -0.3596(7) -1.0403(4) 0.276(4) Uani 1 1 d . D 4 Cl2 Cl 2.1137(3) -0.4003(5) -1.1792(3) 0.201(2) Uani 1 1 d . D 4 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 0.0293(7) 0.1209(14) 0.0941(12) -0.0773(11) -0.0110(7) -0.0017(7) Mn2 0.0262(6) 0.0421(7) 0.0546(8) -0.0168(6) -0.0028(5) -0.0041(5) C1 0.047(5) 0.047(5) 0.075(6) -0.033(5) -0.018(5) 0.005(4) N1 0.034(4) 0.047(4) 0.064(5) -0.023(4) -0.015(3) 0.002(3) N2 0.048(5) 0.267(14) 0.062(6) -0.087(8) -0.011(4) -0.023(6) O1 0.077(6) 0.46(2) 0.086(7) -0.105(10) -0.025(5) -0.018(8) C2 0.041(4) 0.042(5) 0.049(5) -0.012(4) -0.013(4) -0.003(4) O2 0.110(5) 0.048(4) 0.050(4) -0.005(3) -0.021(4) -0.008(4) C3 0.031(5) 0.074(7) 0.204(13) -0.080(8) -0.005(6) -0.009(5) O3 0.029(4) 0.159(8) 0.53(2) -0.239(12) -0.018(7) -0.005(5) P1 0.0501(13) 0.0464(13) 0.0423(13) -0.0102(11) -0.0136(10) -0.0087(11) P2 0.0358(11) 0.0439(13) 0.0455(13) -0.0165(10) -0.0015(9) -0.0071(10) P3 0.104(2) 0.0415(14) 0.0578(16) -0.0205(13) 0.0245(15) -0.0121(14) O4 0.188(8) 0.036(4) 0.063(4) -0.024(4) 0.001(5) 0.003(4) O5 0.048(7) 0.062(8) 0.079(9) -0.015(6) 0.018(8) -0.004(7) O6 0.039(5) 0.076(7) 0.071(7) -0.038(5) 0.007(4) -0.021(5) C4 0.092(8) 0.037(6) 0.049(6) -0.018(5) 0.012(6) 0.006(6) C5 0.079(7) 0.055(7) 0.069(7) -0.024(6) 0.024(6) -0.011(6) C6 0.054(6) 0.055(6) 0.083(7) -0.022(6) 0.018(5) 0.006(5) C7 0.078(7) 0.043(6) 0.067(7) -0.006(5) 0.025(6) -0.003(6) C8 0.070(7) 0.062(7) 0.069(7) -0.030(6) 0.017(6) -0.011(5) C9 0.071(7) 0.062(7) 0.049(6) -0.028(5) 0.004(5) 0.008(6) C10 0.042(8) 0.047(9) 0.073(11) -0.007(8) 0.014(8) -0.020(7) C11 0.057(16) 0.14(2) 0.056(12) -0.014(16) 0.005(11) -0.035(17) C12 0.053(11) 0.17(3) 0.081(15) -0.001(17) 0.029(11) -0.008(13) C13 0.08(2) 0.11(3) 0.13(4) 0.02(2) 0.06(2) 0.005(19) C14 0.091(13) 0.094(13) 0.063(10) -0.032(10) 0.035(10) -0.048(11) C15 0.075(11) 0.069(11) 0.049(10) -0.002(8) 0.009(8) -0.024(8) C16 0.061(10) 0.060(10) 0.044(9) -0.017(8) 0.001(7) -0.014(8) C17 0.071(10) 0.065(10) 0.065(10) -0.025(9) -0.011(8) -0.003(8) C18 0.071(10) 0.086(13) 0.068(11) -0.035(10) -0.015(9) -0.008(9) C19 0.091(15) 0.11(2) 0.071(14) -0.031(14) -0.013(12) -0.018(13) C20 0.078(16) 0.10(2) 0.10(2) -0.007(16) -0.045(15) -0.010(12) C21 0.046(11) 0.083(14) 0.080(17) -0.040(12) -0.006(9) 0.009(10) C22 0.053(12) 0.037(11) 0.022(11) -0.021(9) 0.002(8) -0.015(9) C23 0.058(11) 0.049(11) 0.068(12) 0.002(9) -0.033(10) -0.022(9) C24 0.058(12) 0.080(15) 0.090(16) -0.019(13) -0.020(11) -0.037(12) C25 0.083(18) 0.10(2) 0.11(2) -0.033(16) -0.009(15) -0.074(17) C26 0.107(18) 0.048(13) 0.109(18) -0.030(13) 0.010(15) -0.033(13) C27 0.061(13) 0.047(12) 0.079(15) -0.027(11) 0.010(11) -0.022(10) O5' 0.038(8) 0.044(9) 0.056(10) -0.019(8) 0.002(7) -0.006(7) C10' 0.04(2) 0.015(13) 0.10(4) -0.032(17) -0.003(19) 0.009(13) C11' 0.070(19) 0.054(18) 0.042(18) 0.019(13) 0.012(14) -0.034(16) C12' 0.08(2) 0.05(2) 0.07(2) 0.029(17) 0.008(18) -0.010(18) C13' 0.06(3) 0.06(3) 0.08(4) -0.06(3) 0.00(2) -0.01(2) C14' 0.09(2) 0.09(3) 0.11(3) -0.08(2) 0.000(19) 0.004(19) C15' 0.073(18) 0.049(16) 0.09(2) -0.039(15) 0.050(15) -0.014(13) O6' 0.076(14) 0.024(9) 0.026(9) -0.011(7) -0.030(11) 0.009(11) C16' 0.026(11) 0.044(13) 0.039(13) -0.016(11) 0.005(9) -0.014(10) C17' 0.035(12) 0.12(2) 0.064(16) -0.067(17) 0.023(11) -0.029(13) C18' 0.080(19) 0.11(2) 0.047(15) -0.064(16) 0.016(14) -0.045(17) C19' 0.10(3) 0.06(2) 0.027(17) 0.005(16) -0.033(18) -0.035(19) C20' 0.07(3) 0.25(5) 0.07(3) -0.09(3) -0.01(2) -0.01(3) C21' 0.13(3) 0.13(3) 0.05(2) -0.07(2) -0.03(2) 0.05(3) C28 0.043(13) 0.042(13) 0.043(12) -0.021(11) -0.018(9) -0.003(11) C29 0.066(11) 0.052(12) 0.072(12) -0.021(10) -0.050(10) -0.008(9) C30 0.087(14) 0.067(14) 0.106(16) -0.021(12) -0.076(13) -0.003(11) C31 0.044(11) 0.043(12) 0.077(13) 0.001(10) -0.044(10) 0.000(9) C32 0.083(17) 0.076(19) 0.093(18) -0.023(14) -0.042(14) -0.022(13) C33 0.056(11) 0.055(13) 0.047(11) -0.009(10) -0.019(9) -0.007(10) C22' 0.042(10) 0.048(11) 0.016(11) -0.012(8) -0.006(7) -0.002(8) C23' 0.053(11) 0.061(12) 0.080(13) -0.035(11) 0.000(10) -0.020(9) C24' 0.056(12) 0.075(14) 0.070(13) -0.018(11) -0.004(10) -0.027(10) C25' 0.055(12) 0.081(16) 0.109(18) -0.014(14) -0.007(13) -0.042(11) C26' 0.075(16) 0.076(18) 0.070(15) 0.009(13) -0.043(13) -0.053(15) C27' 0.069(15) 0.080(17) 0.044(12) -0.018(12) -0.007(10) -0.036(13) C28' 0.080(18) 0.033(12) 0.063(18) -0.002(11) -0.047(13) -0.005(11) C29' 0.079(14) 0.082(15) 0.047(12) -0.006(11) -0.026(11) -0.010(11) C30' 0.13(2) 0.094(17) 0.039(12) 0.000(11) -0.023(13) -0.039(15) C31' 0.106(19) 0.061(15) 0.11(2) -0.004(14) -0.074(17) 0.010(13) C32' 0.065(16) 0.066(19) 0.082(18) -0.009(15) -0.040(14) 0.021(15) C33' 0.049(12) 0.055(15) 0.070(16) 0.002(12) -0.025(12) 0.007(12) C34 0.058(5) 0.058(6) 0.045(5) -0.017(5) -0.009(4) -0.009(5) C35 0.079(7) 0.071(7) 0.058(6) -0.020(5) 0.012(5) -0.027(6) C36 0.078(7) 0.099(9) 0.086(8) -0.034(7) 0.011(7) -0.024(7) C37 0.122(10) 0.118(11) 0.045(6) -0.020(7) 0.012(7) -0.058(9) C38 0.132(11) 0.090(9) 0.059(7) -0.014(7) 0.000(7) -0.030(8) C39 0.094(8) 0.075(8) 0.047(6) -0.007(6) 0.010(6) -0.017(6) C40 0.081(7) 0.083(7) 0.036(5) -0.005(5) -0.013(5) -0.044(6) C41 0.107(9) 0.146(11) 0.081(8) -0.084(8) 0.037(7) -0.067(8) C42' 0.171(16) 0.29(3) 0.117(14) -0.164(17) 0.079(11) -0.173(17) C42 0.030(5) 0.091(8) 0.069(6) -0.042(6) -0.012(4) 0.007(5) N3 0.054(5) 0.086(6) 0.078(6) -0.037(5) -0.012(4) -0.001(4) C43 0.187(19) 0.35(3) 0.046(8) -0.038(13) 0.016(10) -0.22(2) C44 0.141(12) 0.201(16) 0.125(12) 0.081(11) -0.098(10) -0.139(13) C45 0.138(11) 0.106(10) 0.115(10) 0.042(8) -0.077(9) -0.088(9) C46 0.142(12) 0.157(12) 0.104(9) -0.103(9) 0.060(9) -0.104(10) C47 0.092(8) 0.111(9) 0.079(8) -0.039(7) 0.008(7) -0.061(8) C48 0.048(6) 0.125(9) 0.107(8) -0.081(8) -0.007(6) -0.013(6) C49 0.036(6) 0.170(12) 0.244(16) -0.172(13) -0.029(8) 0.018(7) C50 0.053(7) 0.245(18) 0.31(2) -0.247(18) 0.065(10) -0.067(9) C51 0.41(3) 0.242(19) 0.100(10) -0.112(12) 0.112(14) -0.26(2) C52 0.165(13) 0.092(9) 0.104(10) 0.022(7) -0.067(9) -0.078(9) C53 0.075(7) 0.115(9) 0.088(8) -0.068(7) -0.017(6) 0.025(6) C54 0.104(10) 0.247(19) 0.41(3) -0.27(2) -0.147(14) 0.069(11) C55 0.069(10) 0.50(4) 0.92(6) -0.63(5) 0.19(2) -0.131(16) C56 0.057(6) 0.077(7) 0.109(9) -0.058(7) -0.019(6) -0.009(5) C57 0.49(4) 0.088(13) 0.23(2) -0.048(14) 0.19(3) -0.043(19) C58 0.51(4) 0.130(15) 0.19(2) -0.114(15) -0.08(2) 0.01(2) C59 0.064(10) 0.29(3) 1.04(8) -0.49(4) -0.07(2) 0.040(13) C60 0.052(5) 0.040(5) 0.035(4) -0.009(4) -0.005(4) -0.003(4) P4 0.088(2) 0.0770(19) 0.0696(18) -0.0350(16) 0.0220(16) -0.0439(17) F1 0.093(5) 0.173(7) 0.110(5) -0.031(5) -0.024(4) -0.035(5) F2 0.081(4) 0.079(4) 0.167(6) -0.059(4) 0.009(4) -0.008(3) F3 0.155(6) 0.128(6) 0.094(5) -0.022(4) 0.009(4) -0.098(5) F4 0.245(9) 0.129(6) 0.080(5) -0.058(4) 0.042(5) -0.083(6) F5 0.109(5) 0.081(4) 0.146(6) -0.042(4) 0.037(4) -0.052(4) F6 0.094(4) 0.129(5) 0.096(4) -0.076(4) -0.003(3) -0.006(4) C99 0.114(13) 0.33(3) 0.28(2) -0.24(2) 0.000(14) -0.031(14) Cl1 0.118(4) 0.558(13) 0.189(5) -0.185(7) 0.028(3) -0.092(5) Cl2 0.105(3) 0.299(7) 0.259(6) -0.196(5) -0.040(3) 0.004(3) _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 N2 1.629(10) . ? Mn1 C42 1.883(10) . ? Mn1 C1 1.938(9) . ? Mn1 C50 2.098(13) . ? Mn1 C49 2.125(12) . ? Mn1 C46 2.131(12) . ? Mn1 C48 2.159(11) . ? Mn1 C47 2.188(12) . ? Mn2 C3 1.742(9) . ? Mn2 C2 1.791(9) . ? Mn2 N1 1.996(7) . ? Mn2 P3 2.202(3) . ? Mn2 P1 2.303(2) . ? Mn2 P2 2.352(2) . ? C1 N1 1.161(9) . ? N2 O1 1.179(12) . ? C2 O2 1.153(9) . ? C3 O3 1.164(10) . ? P1 C34 1.808(9) . ? P1 C40 1.816(9) . ? P1 C60 1.830(7) . ? P1 P2 2.692(3) . ? P2 C28' 1.719(10) . ? P2 C22' 1.784(9) . ? P2 C60 1.825(7) . ? P2 C22 1.869(9) . ? P2 C28 1.925(9) . ? P3 O6' 1.445(18) . ? P3 O4 1.509(6) . ? P3 O5 1.556(14) . ? P3 O6 1.808(9) . ? P3 O5' 1.948(13) . ? O4 C4 1.407(10) . ? O5 C10 1.429(18) . ? O6 C16 1.377(11) . ? C4 C9 1.345(13) . ? C4 C5 1.376(13) . ? C5 C6 1.391(12) . ? C6 C7 1.365(12) . ? C7 C8 1.367(13) . ? C8 C9 1.392(12) . ? C10 C11 1.31(3) . ? C10 C15 1.359(19) . ? C11 C12 1.43(3) . ? C12 C13 1.24(4) . ? C13 C14 1.45(4) . ? C14 C15 1.353(18) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? O5' C10' 1.410(18) . ? C10' C11' 1.3900 . ? C10' C15' 1.3900 . ? C11' C12' 1.3900 . ? C12' C13' 1.3900 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? O6' C16' 1.40(2) . ? C16' C17' 1.3900 . ? C16' C21' 1.3900 . ? C17' C18' 1.3900 . ? C18' C19' 1.3900 . ? C19' C20' 1.3900 . ? C20' C21' 1.3900 . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C22' C23' 1.3900 . ? C22' C27' 1.3900 . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? C26' C27' 1.3900 . ? C28' C29' 1.3900 . ? C28' C33' 1.3900 . ? C29' C30' 1.3900 . ? C30' C31' 1.3900 . ? C31' C32' 1.3900 . ? C32' C33' 1.3900 . ? C34 C39 1.384(12) . ? C34 C35 1.385(11) . ? C35 C36 1.402(12) . ? C36 C37 1.394(14) . ? C37 C38 1.382(14) . ? C38 C39 1.388(13) . ? C40 C41 1.364(13) . ? C40 C45 1.387(14) . ? C41 C42' 1.391(17) . ? C42' C43 1.31(3) . ? C42 N3 1.150(10) . ? N3 C56 1.480(12) . ? C43 C44 1.36(3) . ? C44 C45 1.388(15) . ? C46 C47 1.406(15) . ? C46 C50 1.44(2) . ? C46 C51 1.502(15) . ? C47 C48 1.408(13) . ? C47 C52 1.507(15) . ? C48 C49 1.409(12) . ? C48 C53 1.516(12) . ? C49 C50 1.374(17) . ? C49 C54 1.518(17) . ? C50 C55 1.508(16) . ? C56 C57 1.384(18) . ? C56 C59 1.413(17) . ? C56 C58 1.420(19) . ? P4 F6 1.553(6) . ? P4 F5 1.567(6) . ? P4 F2 1.579(7) . ? P4 F4 1.587(6) . ? P4 F3 1.589(6) . ? P4 F1 1.615(7) . ? C99 Cl2 1.614(15) . ? C99 Cl1 1.657(17) . ? 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 N2 Mn1 C42 97.2(5) . . ? N2 Mn1 C1 99.7(4) . . ? C42 Mn1 C1 90.5(3) . . ? N2 Mn1 C50 118.1(6) . . ? C42 Mn1 C50 90.8(4) . . ? C1 Mn1 C50 141.7(6) . . ? N2 Mn1 C49 91.7(6) . . ? C42 Mn1 C49 122.8(4) . . ? C1 Mn1 C49 143.2(4) . . ? C50 Mn1 C49 38.0(5) . . ? N2 Mn1 C46 156.4(5) . . ? C42 Mn1 C46 92.4(4) . . ? C1 Mn1 C46 101.8(5) . . ? C50 Mn1 C46 39.9(6) . . ? C49 Mn1 C46 65.0(5) . . ? N2 Mn1 C48 100.9(5) . . ? C42 Mn1 C48 153.8(4) . . ? C1 Mn1 C48 104.9(3) . . ? C50 Mn1 C48 64.0(4) . . ? C49 Mn1 C48 38.4(3) . . ? C46 Mn1 C48 64.1(4) . . ? N2 Mn1 C47 136.4(5) . . ? C42 Mn1 C47 126.3(4) . . ? C1 Mn1 C47 84.5(4) . . ? C50 Mn1 C47 64.4(6) . . ? C49 Mn1 C47 64.0(5) . . ? C46 Mn1 C47 38.0(4) . . ? C48 Mn1 C47 37.8(4) . . ? C3 Mn2 C2 88.7(4) . . ? C3 Mn2 N1 177.9(4) . . ? C2 Mn2 N1 90.8(3) . . ? C3 Mn2 P3 88.3(4) . . ? C2 Mn2 P3 96.9(3) . . ? N1 Mn2 P3 89.8(2) . . ? C3 Mn2 P1 95.7(4) . . ? C2 Mn2 P1 94.6(3) . . ? N1 Mn2 P1 86.36(19) . . ? P3 Mn2 P1 167.98(10) . . ? C3 Mn2 P2 96.1(3) . . ? C2 Mn2 P2 164.8(3) . . ? N1 Mn2 P2 84.82(19) . . ? P3 Mn2 P2 97.66(9) . . ? P1 Mn2 P2 70.67(8) . . ? N1 C1 Mn1 176.6(7) . . ? C1 N1 Mn2 176.0(6) . . ? O1 N2 Mn1 173.8(10) . . ? O2 C2 Mn2 174.9(7) . . ? O3 C3 Mn2 176.2(12) . . ? C34 P1 C40 104.5(4) . . ? C34 P1 C60 109.1(4) . . ? C40 P1 C60 106.3(4) . . ? C34 P1 Mn2 121.7(3) . . ? C40 P1 Mn2 119.7(3) . . ? C60 P1 Mn2 93.7(2) . . ? C34 P1 P2 142.4(3) . . ? C40 P1 P2 107.4(3) . . ? C60 P1 P2 42.5(2) . . ? Mn2 P1 P2 55.52(7) . . ? C28' P2 C22' 92.1(7) . . ? C28' P2 C60 114.1(6) . . ? C22' P2 C60 115.8(5) . . ? C28' P2 C22 104.3(6) . . ? C22' P2 C22 18.3(4) . . ? C60 P2 C22 98.1(4) . . ? C28' P2 C28 16.0(6) . . ? C22' P2 C28 100.2(6) . . ? C60 P2 C28 98.1(5) . . ? C22 P2 C28 108.4(5) . . ? C28' P2 Mn2 124.9(5) . . ? C22' P2 Mn2 119.6(4) . . ? C60 P2 Mn2 92.2(2) . . ? C22 P2 Mn2 119.4(3) . . ? C28 P2 Mn2 128.9(4) . . ? C28' P2 P1 148.8(5) . . ? C22' P2 P1 115.8(4) . . ? C60 P2 P1 42.6(2) . . ? C22 P2 P1 100.2(3) . . ? C28 P2 P1 134.8(5) . . ? Mn2 P2 P1 53.81(7) . . ? O6' P3 O4 113.1(7) . . ? O6' P3 O5 30.1(7) . . ? O4 P3 O5 104.9(6) . . ? O6' P3 O6 70.2(9) . . ? O4 P3 O6 89.6(4) . . ? O5 P3 O6 98.7(6) . . ? O6' P3 O5' 90.3(9) . . ? O4 P3 O5' 75.3(4) . . ? O5 P3 O5' 60.4(6) . . ? O6 P3 O5' 148.5(5) . . ? O6' P3 Mn2 121.2(7) . . ? O4 P3 Mn2 125.6(3) . . ? O5 P3 Mn2 119.8(6) . . ? O6 P3 Mn2 110.9(3) . . ? O5' P3 Mn2 100.3(4) . . ? C4 O4 P3 129.3(5) . . ? C10 O5 P3 128.3(11) . . ? C16 O6 P3 123.3(7) . . ? C9 C4 C5 122.0(9) . . ? C9 C4 O4 120.4(11) . . ? C5 C4 O4 117.5(11) . . ? C4 C5 C6 118.6(10) . . ? C7 C6 C5 120.3(10) . . ? C6 C7 C8 119.6(9) . . ? C7 C8 C9 120.7(10) . . ? C4 C9 C8 118.7(10) . . ? C11 C10 C15 122.6(18) . . ? C11 C10 O5 114.1(18) . . ? C15 C10 O5 123.0(14) . . ? C10 C11 C12 116(2) . . ? C13 C12 C11 123(3) . . ? C12 C13 C14 119(2) . . ? C15 C14 C13 118(2) . . ? C14 C15 C10 119.5(16) . . ? O6 C16 C17 121.3(9) . . ? O6 C16 C21 118.7(9) . . ? C17 C16 C21 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C16 120.0 . . ? C23 C22 C27 120.0 . . ? C23 C22 P2 123.8(4) . . ? C27 C22 P2 116.1(4) . . ? C24 C23 C22 120.0 . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C22 120.0 . . ? C10' O5' P3 121.8(13) . . ? C11' C10' C15' 120.0 . . ? C11' C10' O5' 119.6(11) . . ? C15' C10' O5' 120.0(12) . . ? C12' C11' C10' 120.0 . . ? C11' C12' C13' 120.0 . . ? C14' C13' C12' 120.0 . . ? C13' C14' C15' 120.0 . . ? C14' C15' C10' 120.0 . . ? C16' O6' P3 121.1(16) . . ? C17' C16' C21' 120.0 . . ? C17' C16' O6' 120.1(13) . . ? C21' C16' O6' 119.7(13) . . ? C16' C17' C18' 120.0 . . ? C17' C18' C19' 120.0 . . ? C20' C19' C18' 120.0 . . ? C19' C20' C21' 120.0 . . ? C20' C21' C16' 120.0 . . ? C29 C28 C33 120.0 . . ? C29 C28 P2 119.8(7) . . ? C33 C28 P2 119.8(7) . . ? C30 C29 C28 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C28 120.0 . . ? C23' C22' C27' 120.0 . . ? C23' C22' P2 118.6(7) . . ? C27' C22' P2 121.4(7) . . ? C22' C23' C24' 120.0 . . ? C23' C24' C25' 120.0 . . ? C26' C25' C24' 120.0 . . ? C25' C26' C27' 120.0 . . ? C26' C27' C22' 120.0 . . ? C29' C28' C33' 120.0 . . ? C29' C28' P2 117.6(9) . . ? C33' C28' P2 122.3(9) . . ? C28' C29' C30' 120.0 . . ? C31' C30' C29' 120.0 . . ? C32' C31' C30' 120.0 . . ? C33' C32' C31' 120.0 . . ? C32' C33' C28' 120.0 . . ? C39 C34 C35 118.8(8) . . ? C39 C34 P1 119.0(7) . . ? C35 C34 P1 122.2(7) . . ? C34 C35 C36 120.9(9) . . ? C37 C36 C35 119.1(10) . . ? C38 C37 C36 120.2(10) . . ? C37 C38 C39 119.7(11) . . ? C34 C39 C38 121.3(10) . . ? C41 C40 C45 117.7(10) . . ? C41 C40 P1 124.3(9) . . ? C45 C40 P1 118.0(8) . . ? C40 C41 C42' 119.9(14) . . ? C43 C42' C41 121.0(19) . . ? N3 C42 Mn1 176.2(8) . . ? C42 N3 C56 173.1(9) . . ? C42' C43 C44 121.8(17) . . ? C43 C44 C45 118.1(15) . . ? C40 C45 C44 121.3(13) . . ? C47 C46 C50 106.7(9) . . ? C47 C46 C51 125.7(16) . . ? C50 C46 C51 127.5(14) . . ? C47 C46 Mn1 73.2(6) . . ? C50 C46 Mn1 68.8(8) . . ? C51 C46 Mn1 125.3(8) . . ? C46 C47 C48 108.0(11) . . ? C46 C47 C52 127.0(12) . . ? C48 C47 C52 125.0(10) . . ? C46 C47 Mn1 68.8(7) . . ? C48 C47 Mn1 70.0(7) . . ? C52 C47 Mn1 128.5(7) . . ? C47 C48 C49 108.4(10) . . ? C47 C48 C53 125.3(9) . . ? C49 C48 C53 126.2(10) . . ? C47 C48 Mn1 72.2(6) . . ? C49 C48 Mn1 69.5(6) . . ? C53 C48 Mn1 126.2(8) . . ? C50 C49 C48 108.3(12) . . ? C50 C49 C54 126.6(11) . . ? C48 C49 C54 125.0(10) . . ? C50 C49 Mn1 70.0(7) . . ? C48 C49 Mn1 72.1(6) . . ? C54 C49 Mn1 125.5(12) . . ? C49 C50 C46 108.6(10) . . ? C49 C50 C55 127.2(18) . . ? C46 C50 C55 124.1(17) . . ? C49 C50 Mn1 72.1(8) . . ? C46 C50 Mn1 71.3(6) . . ? C55 C50 Mn1 126.0(13) . . ? C57 C56 C59 112.8(19) . . ? C57 C56 C58 111.7(16) . . ? C59 C56 C58 104.2(19) . . ? C57 C56 N3 112.3(11) . . ? C59 C56 N3 106.6(9) . . ? C58 C56 N3 108.8(10) . . ? P2 C60 P1 94.9(3) . . ? F6 P4 F5 91.2(4) . . ? F6 P4 F2 90.5(4) . . ? F5 P4 F2 90.3(4) . . ? F6 P4 F4 179.0(4) . . ? F5 P4 F4 89.4(4) . . ? F2 P4 F4 90.3(4) . . ? F6 P4 F3 90.4(4) . . ? F5 P4 F3 178.3(4) . . ? F2 P4 F3 89.2(4) . . ? F4 P4 F3 88.9(4) . . ? F6 P4 F1 89.7(4) . . ? F5 P4 F1 90.1(4) . . ? F2 P4 F1 179.5(4) . . ? F4 P4 F1 89.5(4) . . ? F3 P4 F1 90.4(4) . . ? Cl2 C99 Cl1 116.4(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.637 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.081 #===END data_cis-12[PF6] _database_code_depnum_ccdc_archive 'CCDC 644604' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H59 F6 Mn2 N2 O9 P5' _chemical_formula_weight 1450.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 34.821(3) _cell_length_b 11.1610(11) _cell_length_c 37.628(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14624(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 178 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.001 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5952 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632785 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 89374 _diffrn_reflns_av_R_equivalents 0.1414 _diffrn_reflns_av_sigmaI/netI 0.2469 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.51 _reflns_number_total 31246 _reflns_number_gt 11777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.689(19) _refine_ls_number_reflns 31246 _refine_ls_number_parameters 1660 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1874 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.003 _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 Mn2 Mn -0.06632(3) -0.17552(11) -0.14836(3) 0.044 Uani 1 1 d . . . Mn1 Mn 0.06854(3) -0.32177(10) -0.17319(2) 0.0314(3) Uani 1 1 d . . . P1 P 0.08878(5) -0.21816(17) -0.12300(4) 0.0332(5) Uani 1 1 d . . . P2 P 0.06319(5) -0.44875(17) -0.12556(4) 0.0326(5) Uani 1 1 d . . . P3 P 0.07574(5) -0.16935(18) -0.20954(4) 0.0339(5) Uani 1 1 d . . . P4 P -0.08453(5) -0.2788(2) -0.19581(5) 0.0490(6) Uani 1 1 d . . . O1 O -0.05956(15) 0.0549(6) -0.17805(13) 0.0775(19) Uani 1 1 d . . . O2 O 0.03986(15) -0.4950(5) -0.22523(12) 0.0611(16) Uani 1 1 d . . . O3 O 0.14712(12) -0.3936(5) -0.19332(12) 0.0534(15) Uani 1 1 d . . . O4 O -0.12718(12) -0.2628(5) -0.21147(11) 0.0497(14) Uani 1 1 d . . . O5 O -0.06014(14) -0.2646(6) -0.23166(13) 0.0710(18) Uani 1 1 d . . . O6 O -0.08184(14) -0.4172(5) -0.18836(12) 0.0592(16) Uani 1 1 d . . . O7 O 0.03801(12) -0.0907(4) -0.21596(10) 0.0380(12) Uani 1 1 d . . . O8 O 0.09348(12) -0.1881(4) -0.24895(10) 0.0401(12) Uani 1 1 d . . . O9 O 0.10659(12) -0.0758(4) -0.19563(10) 0.0411(13) Uani 1 1 d . . . N1 N -0.01605(17) -0.2422(5) -0.15648(13) 0.0420(16) Uani 1 1 d . . . N2 N -0.06015(16) -0.0469(6) -0.16701(15) 0.0558(19) Uani 1 1 d . . . C1 C 0.0159(2) -0.2718(6) -0.16235(15) 0.0332(17) Uani 1 1 d . . . C2 C 0.05063(19) -0.4263(6) -0.20543(16) 0.0344(18) Uani 1 1 d . . . C3 C 0.11683(18) -0.3656(6) -0.18406(15) 0.0322(18) Uani 1 1 d . . . C4 C -0.0831(2) 0.0397(8) -0.0920(2) 0.075(3) Uani 1 1 d . . . H1A H -0.0949 0.0544 -0.0687 0.112 Uiso 1 1 calc R . . H1B H -0.0966 0.0862 -0.1102 0.112 Uiso 1 1 calc R . . H1C H -0.0561 0.0639 -0.0913 0.112 Uiso 1 1 calc R . . C5 C -0.08570(18) -0.0898(7) -0.10061(17) 0.043(2) Uani 1 1 d . . . C6 C -0.0590(2) -0.1827(9) -0.09258(17) 0.061(3) Uani 1 1 d . . . H6A H -0.0347 -0.1710 -0.0816 0.073 Uiso 1 1 calc R . . C7 C -0.0736(2) -0.2915(7) -0.10303(19) 0.060(3) Uani 1 1 d . . . H5A H -0.0614 -0.3669 -0.1000 0.072 Uiso 1 1 calc R . . C8 C -0.1083(2) -0.2728(8) -0.1184(2) 0.071(3) Uani 1 1 d . . . H4A H -0.1244 -0.3329 -0.1284 0.085 Uiso 1 1 calc R . . C9 C -0.1167(2) -0.1491(8) -0.11703(17) 0.058(2) Uani 1 1 d . . . H3A H -0.1394 -0.1121 -0.1257 0.070 Uiso 1 1 calc R . . C10 C -0.1537(2) -0.1738(8) -0.19965(17) 0.052(2) Uani 1 1 d . . . C11 C -0.1440(2) -0.0572(8) -0.2046(2) 0.067(3) Uani 1 1 d . . . H17A H -0.1206 -0.0363 -0.2160 0.080 Uiso 1 1 calc R . . C12 C -0.1684(3) 0.0294(10) -0.1927(2) 0.091(3) Uani 1 1 d . . . H16A H -0.1623 0.1119 -0.1954 0.109 Uiso 1 1 calc R . . C13 C -0.2018(3) -0.0053(12) -0.1770(2) 0.116(5) Uani 1 1 d . . . H15A H -0.2186 0.0547 -0.1682 0.139 Uiso 1 1 calc R . . C14 C -0.2121(2) -0.1216(10) -0.1734(2) 0.081(3) Uani 1 1 d . . . H14A H -0.2362 -0.1434 -0.1636 0.097 Uiso 1 1 calc R . . C15 C -0.1859(2) -0.2078(10) -0.18449(17) 0.077(3) Uani 1 1 d . . . H13A H -0.1912 -0.2905 -0.1812 0.093 Uiso 1 1 calc R . . C16 C -0.0694(2) -0.1904(9) -0.26070(19) 0.063(3) Uani 1 1 d . . . C17 C -0.0535(2) -0.0845(9) -0.2641(2) 0.074(3) Uani 1 1 d . . . H23A H -0.0366 -0.0579 -0.2459 0.088 Uiso 1 1 calc R . . C18 C -0.0602(3) -0.0087(11) -0.2929(3) 0.111(4) Uani 1 1 d . . . H22 H -0.0480 0.0672 -0.2947 0.133 Uiso 1 1 calc R . . C19 C -0.0841(3) -0.0472(19) -0.3175(3) 0.231(14) Uani 1 1 d . . . H21A H -0.0893 0.0004 -0.3379 0.277 Uiso 1 1 calc R . . C20 C -0.1009(3) -0.1524(18) -0.3137(3) 0.227(12) Uani 1 1 d . . . H20A H -0.1197 -0.1740 -0.3308 0.272 Uiso 1 1 calc R . . C21 C -0.0932(3) -0.2378(12) -0.2856(2) 0.134(6) Uani 1 1 d . . . H19 H -0.1035 -0.3166 -0.2847 0.161 Uiso 1 1 calc R . . C22 C -0.0907(2) -0.5086(8) -0.21379(18) 0.058(2) Uani 1 1 d . . . C23 C -0.1252(3) -0.5605(7) -0.2125(2) 0.073(3) Uani 1 1 d . . . H11A H -0.1445 -0.5305 -0.1971 0.087 Uiso 1 1 calc R . . C24 C -0.1324(3) -0.6582(9) -0.2339(2) 0.093(4) Uani 1 1 d . . . H10A H -0.1570 -0.6949 -0.2327 0.111 Uiso 1 1 calc R . . C25 C -0.1058(3) -0.7043(9) -0.2565(2) 0.091(4) Uani 1 1 d . . . H9A H -0.1112 -0.7745 -0.2699 0.110 Uiso 1 1 calc R . . C26 C -0.0703(3) -0.6456(10) -0.2596(3) 0.125(5) Uani 1 1 d . . . H8A H -0.0525 -0.6695 -0.2774 0.149 Uiso 1 1 calc R . . C27 C -0.0609(2) -0.5489(9) -0.2357(2) 0.089(4) Uani 1 1 d . . . H7A H -0.0359 -0.5146 -0.2349 0.106 Uiso 1 1 calc R . . C28 C 0.0364(2) 0.0221(6) -0.23412(16) 0.0376(19) Uani 1 1 d . . . C29 C 0.0259(2) 0.1195(7) -0.2135(2) 0.050(2) Uani 1 1 d . . . H35A H 0.0209 0.1109 -0.1888 0.061 Uiso 1 1 calc R . . C30 C 0.0229(2) 0.2287(8) -0.2299(2) 0.060(2) Uani 1 1 d . . . H34A H 0.0142 0.2950 -0.2163 0.072 Uiso 1 1 calc R . . C31 C 0.0319(2) 0.2470(7) -0.26531(19) 0.065(3) Uani 1 1 d . . . H33A H 0.0306 0.3243 -0.2758 0.079 Uiso 1 1 calc R . . C32 C 0.0427(2) 0.1491(7) -0.28426(18) 0.064(3) Uani 1 1 d . . . H32A H 0.0480 0.1588 -0.3088 0.077 Uiso 1 1 calc R . . C33 C 0.0462(2) 0.0365(7) -0.26975(17) 0.056(2) Uani 1 1 d . . . H31A H 0.0550 -0.0292 -0.2836 0.067 Uiso 1 1 calc R . . C34 C 0.0754(2) -0.2560(7) -0.27625(17) 0.045(2) Uani 1 1 d . . . C35 C 0.0371(2) -0.2820(7) -0.27722(19) 0.054(2) Uani 1 1 d . . . H41A H 0.0207 -0.2551 -0.2587 0.065 Uiso 1 1 calc R . . C36 C 0.0222(3) -0.3486(7) -0.30571(19) 0.065(3) Uani 1 1 d . . . H40A H -0.0041 -0.3711 -0.3068 0.078 Uiso 1 1 calc R . . C37 C 0.0491(3) -0.3809(10) -0.3333(3) 0.103(4) Uani 1 1 d . . . H39A H 0.0401 -0.4250 -0.3532 0.123 Uiso 1 1 calc R . . C38 C 0.0843(3) -0.3527(8) -0.3321(2) 0.090(4) Uani 1 1 d . . . H38A H 0.1006 -0.3763 -0.3511 0.108 Uiso 1 1 calc R . . C39 C 0.1000(2) -0.2884(8) -0.30387(19) 0.070(3) Uani 1 1 d . . . H37A H 0.1264 -0.2674 -0.3035 0.083 Uiso 1 1 calc R . . C40 C 0.1374(2) -0.0149(8) -0.21403(17) 0.049(2) Uani 1 1 d . . . C41 C 0.1715(2) -0.0706(8) -0.21464(19) 0.060(2) Uani 1 1 d . . . H29A H 0.1744 -0.1490 -0.2052 0.072 Uiso 1 1 calc R . . C42 C 0.2038(2) -0.0080(9) -0.2301(2) 0.073(3) Uani 1 1 d . . . H28A H 0.2281 -0.0458 -0.2330 0.087 Uiso 1 1 calc R . . C43 C 0.1982(3) 0.1036(10) -0.2402(2) 0.084(4) Uani 1 1 d . . . H27A H 0.2194 0.1474 -0.2493 0.101 Uiso 1 1 calc R . . C44 C 0.1634(3) 0.1594(9) -0.2382(2) 0.080(3) Uani 1 1 d . . . H26A H 0.1607 0.2404 -0.2455 0.096 Uiso 1 1 calc R . . C45 C 0.1325(2) 0.0968(7) -0.22548(17) 0.055(2) Uani 1 1 d . . . H25A H 0.1078 0.1328 -0.2249 0.066 Uiso 1 1 calc R . . C46 C 0.07398(17) -0.3360(6) -0.09276(16) 0.0362(17) Uani 1 1 d . . . H49A H 0.0950 -0.3609 -0.0766 0.043 Uiso 1 1 calc R . . H49B H 0.0511 -0.3133 -0.0787 0.043 Uiso 1 1 calc R . . C47 C 0.14005(18) -0.1966(6) -0.11750(15) 0.0358(18) Uani 1 1 d . . . C48 C 0.1642(2) -0.2963(8) -0.11140(18) 0.058(2) Uani 1 1 d . . . H54A H 0.1535 -0.3734 -0.1075 0.070 Uiso 1 1 calc R . . C49 C 0.2035(2) -0.2804(8) -0.11122(17) 0.058(2) Uani 1 1 d . . . H53A H 0.2197 -0.3476 -0.1073 0.069 Uiso 1 1 calc R . . C50 C 0.21976(19) -0.1696(8) -0.11659(18) 0.054(2) Uani 1 1 d . . . H52A H 0.2469 -0.1600 -0.1165 0.065 Uiso 1 1 calc R . . C51 C 0.19626(19) -0.0739(8) -0.12204(18) 0.057(2) Uani 1 1 d . . . H51A H 0.2074 0.0031 -0.1252 0.068 Uiso 1 1 calc R . . C52 C 0.15684(18) -0.0851(6) -0.12309(16) 0.0405(18) Uani 1 1 d . . . H50A H 0.1412 -0.0170 -0.1276 0.049 Uiso 1 1 calc R . . C53 C 0.06950(18) -0.0837(6) -0.10424(17) 0.0361(18) Uani 1 1 d . . . C54 C 0.0778(2) -0.0507(8) -0.0686(2) 0.057(2) Uani 1 1 d . . . H69A H 0.0934 -0.1011 -0.0543 0.068 Uiso 1 1 calc R . . C55 C 0.0634(2) 0.0531(7) -0.0549(2) 0.061(2) Uani 1 1 d . . . H68A H 0.0692 0.0742 -0.0310 0.073 Uiso 1 1 calc R . . C56 C 0.0410(2) 0.1264(8) -0.0745(2) 0.064(3) Uani 1 1 d . . . H67A H 0.0320 0.1998 -0.0648 0.077 Uiso 1 1 calc R . . C57 C 0.0317(3) 0.0945(7) -0.1078(2) 0.076(3) Uani 1 1 d . . . H66A H 0.0149 0.1449 -0.1210 0.092 Uiso 1 1 calc R . . C58 C 0.04533(19) -0.0076(7) -0.12346(18) 0.046(2) Uani 1 1 d . . . H65A H 0.0384 -0.0266 -0.1472 0.055 Uiso 1 1 calc R . . C59 C 0.01822(17) -0.5149(7) -0.11265(15) 0.0363(19) Uani 1 1 d . . . C60 C 0.00779(19) -0.5288(7) -0.07701(17) 0.048(2) Uani 1 1 d . . . H47A H 0.0243 -0.4989 -0.0590 0.058 Uiso 1 1 calc R . . C61 C -0.02651(17) -0.5860(6) -0.06741(17) 0.041(2) Uani 1 1 d . . . H46A H -0.0330 -0.5957 -0.0430 0.050 Uiso 1 1 calc R . . C62 C -0.05076(19) -0.6282(7) -0.09333(18) 0.047(2) Uani 1 1 d . . . H45A H -0.0741 -0.6659 -0.0866 0.056 Uiso 1 1 calc R . . C63 C -0.0419(2) -0.6168(7) -0.1291(2) 0.058(2) Uani 1 1 d . . . H44A H -0.0589 -0.6463 -0.1468 0.069 Uiso 1 1 calc R . . C64 C -0.00707(19) -0.5604(6) -0.13869(17) 0.045(2) Uani 1 1 d . . . H43A H -0.0005 -0.5530 -0.1631 0.054 Uiso 1 1 calc R . . C65 C 0.09670(18) -0.5671(6) -0.11818(16) 0.0361(18) Uani 1 1 d . . . C66 C 0.1088(2) -0.6391(6) -0.14602(19) 0.050(2) Uani 1 1 d . . . H63A H 0.0997 -0.6232 -0.1693 0.060 Uiso 1 1 calc R . . C67 C 0.1343(3) -0.7354(8) -0.1406(2) 0.084(3) Uani 1 1 d . . . H62A H 0.1436 -0.7804 -0.1602 0.100 Uiso 1 1 calc R . . C68 C 0.1457(2) -0.7636(8) -0.1068(2) 0.073(3) Uani 1 1 d . . . H61A H 0.1611 -0.8325 -0.1028 0.088 Uiso 1 1 calc R . . C69 C 0.1350(2) -0.6937(7) -0.0789(2) 0.060(2) Uani 1 1 d . . . H60A H 0.1446 -0.7088 -0.0557 0.072 Uiso 1 1 calc R . . C70 C 0.1100(2) -0.6008(7) -0.08504(18) 0.049(2) Uani 1 1 d . . . H59A H 0.1013 -0.5565 -0.0651 0.059 Uiso 1 1 calc R . . Mn102 Mn 0.21381(3) 0.16880(11) 0.03798(2) 0.0411(3) Uani 1 1 d . . . Mn101 Mn 0.34404(3) 0.33718(10) 0.07197(2) 0.0336(3) Uani 1 1 d . . . P101 P 0.36301(5) 0.25323(18) 0.01752(4) 0.0315(5) Uani 1 1 d . . . P102 P 0.33619(5) 0.48033(17) 0.02918(4) 0.0330(5) Uani 1 1 d . . . P103 P 0.35196(5) 0.17971(18) 0.10670(4) 0.0346(5) Uani 1 1 d . . . P104 P 0.19291(5) 0.2317(2) 0.09004(5) 0.0527(6) Uani 1 1 d . . . O101 O 0.22324(15) -0.0733(6) 0.05750(13) 0.073 Uani 1 1 d . . . O102 O 0.31347(14) 0.5049(4) 0.12562(11) 0.051 Uani 1 1 d . . . O103 O 0.42213(14) 0.4182(5) 0.09310(13) 0.059 Uani 1 1 d . . . O104 O 0.15346(13) 0.1874(6) 0.10641(11) 0.083 Uani 1 1 d . . . O105 O 0.22112(13) 0.2058(5) 0.12332(11) 0.060 Uani 1 1 d . . . O106 O 0.18982(16) 0.3748(5) 0.09099(12) 0.072 Uani 1 1 d . . . O107 O 0.31428(12) 0.1021(4) 0.11291(10) 0.039 Uani 1 1 d . . . O108 O 0.38243(12) 0.0769(4) 0.09487(11) 0.046 Uani 1 1 d . . . O109 O 0.36857(11) 0.2007(4) 0.14687(9) 0.031 Uani 1 1 d . . . N101 N 0.26252(15) 0.2395(5) 0.05108(12) 0.0362(16) Uani 1 1 d . . . N102 N 0.22058(16) 0.0308(6) 0.05077(14) 0.0494(17) Uani 1 1 d . . . C101 C 0.29213(18) 0.2760(6) 0.05889(14) 0.0269(17) Uani 1 1 d . . . C103 C 0.3919(2) 0.3862(6) 0.08429(17) 0.0410(19) Uani 1 1 d . . . C102 C 0.32543(19) 0.4337(6) 0.10564(17) 0.0398(18) Uani 1 1 d . . . C104 C 0.1847(3) -0.0218(9) -0.0221(2) 0.091(3) Uani 1 1 d . . . H10B H 0.1694 -0.0243 -0.0440 0.137 Uiso 1 1 calc R . . H10C H 0.1714 -0.0666 -0.0034 0.137 Uiso 1 1 calc R . . H10D H 0.2099 -0.0578 -0.0265 0.137 Uiso 1 1 calc R . . C105 C 0.1897(2) 0.1051(8) -0.01073(17) 0.056(2) Uani 1 1 d . . . C106 C 0.2221(2) 0.1783(9) -0.01875(16) 0.060(3) Uani 1 1 d . . . H10E H 0.2449 0.1534 -0.0304 0.072 Uiso 1 1 calc R . . C107 C 0.2139(2) 0.2946(9) -0.0061(2) 0.074(3) Uani 1 1 d . . . H10F H 0.2303 0.3623 -0.0084 0.089 Uiso 1 1 calc R . . C108 C 0.1789(3) 0.2945(9) 0.00998(18) 0.076(3) Uani 1 1 d . . . H10G H 0.1673 0.3618 0.0210 0.091 Uiso 1 1 calc R . . C109 C 0.1620(2) 0.1750(9) 0.00763(17) 0.069(3) Uani 1 1 d . . . H10H H 0.1378 0.1497 0.0164 0.082 Uiso 1 1 calc R . . C110 C 0.12565(15) 0.1347(7) 0.08803(13) 0.079(3) Uani 1 1 d G . . C111 C 0.1270(2) 0.0114(7) 0.08299(17) 0.134(5) Uani 1 1 d G . . H11B H 0.1481 -0.0335 0.0920 0.160 Uiso 1 1 calc R . . C112 C 0.0976(3) -0.0463(6) 0.06479(19) 0.203(10) Uani 1 1 d G . . H110 H 0.0986 -0.1305 0.0613 0.243 Uiso 1 1 calc R . . C113 C 0.0668(2) 0.0194(10) 0.05163(16) 0.219(14) Uani 1 1 d G . . H10K H 0.0467 -0.0200 0.0392 0.263 Uiso 1 1 calc R . . C114 C 0.06544(14) 0.1427(10) 0.05667(15) 0.213(11) Uani 1 1 d G . . H10J H 0.0444 0.1876 0.0477 0.256 Uiso 1 1 calc R . . C115 C 0.0949(2) 0.2003(6) 0.07487(15) 0.111(4) Uani 1 1 d G . . H10I H 0.0939 0.2846 0.0783 0.134 Uiso 1 1 calc R . . C116 C 0.21396(15) 0.1357(5) 0.15227(11) 0.065(3) Uani 1 1 d G . . C117 C 0.21503(15) 0.0113(6) 0.15076(12) 0.079(3) Uani 1 1 d G . . H12G H 0.2205 -0.0278 0.1289 0.095 Uiso 1 1 calc R . . C118 C 0.20811(16) -0.0558(5) 0.18121(18) 0.104(4) Uani 1 1 d G . . H122 H 0.2088 -0.1408 0.1802 0.125 Uiso 1 1 calc R . . C119 C 0.20012(16) 0.0014(7) 0.21317(13) 0.127(6) Uani 1 1 d G . . H121 H 0.1954 -0.0445 0.2340 0.152 Uiso 1 1 calc R . . C120 C 0.19904(17) 0.1258(7) 0.21468(11) 0.130(6) Uani 1 1 d G . . H12F H 0.1936 0.1649 0.2365 0.156 Uiso 1 1 calc R . . C121 C 0.20596(17) 0.1929(5) 0.18423(15) 0.094(4) Uani 1 1 d G . . H119 H 0.2052 0.2780 0.1853 0.113 Uiso 1 1 calc R . . C122 C 0.18524(18) 0.4393(7) 0.12146(15) 0.093(3) Uani 1 1 d G . . C123 C 0.21651(13) 0.4852(6) 0.13997(15) 0.079(3) Uani 1 1 d G . . H12H H 0.2419 0.4675 0.1323 0.095 Uiso 1 1 calc R . . C124 C 0.21064(17) 0.5570(7) 0.16967(16) 0.099(4) Uani 1 1 d G . . H12I H 0.2320 0.5883 0.1823 0.118 Uiso 1 1 calc R . . C125 C 0.1735(2) 0.5828(9) 0.1809(2) 0.209(9) Uani 1 1 d G . . H12J H 0.1695 0.6319 0.2012 0.251 Uiso 1 1 calc R . . C126 C 0.14226(15) 0.5370(11) 0.1624(3) 0.47(3) Uani 1 1 d G . . H12K H 0.1169 0.5546 0.1700 0.568 Uiso 1 1 calc R . . C127 C 0.14812(15) 0.4652(9) 0.1327(2) 0.238(11) Uani 1 1 d G . . H12L H 0.1268 0.4339 0.1200 0.285 Uiso 1 1 calc R . . C128 C 0.31200(19) -0.0108(6) 0.12911(18) 0.0397(19) Uani 1 1 d . . . C129 C 0.3170(2) -0.0238(7) 0.16531(18) 0.051(2) Uani 1 1 d . . . H12E H 0.3240 0.0435 0.1794 0.061 Uiso 1 1 calc R . . C130 C 0.3120(2) -0.1326(6) 0.18074(19) 0.050(2) Uani 1 1 d . . . H12D H 0.3161 -0.1416 0.2056 0.060 Uiso 1 1 calc R . . C131 C 0.3014(2) -0.2275(7) 0.16124(18) 0.050(2) Uani 1 1 d . . . H12B H 0.2981 -0.3032 0.1724 0.060 Uiso 1 1 calc R . . C132 C 0.2952(2) -0.2166(7) 0.12577(19) 0.059(2) Uani 1 1 d . . . H12A H 0.2874 -0.2845 0.1124 0.071 Uiso 1 1 calc R . . C133 C 0.3002(2) -0.1068(7) 0.1089(2) 0.049(2) Uani 1 1 d . . . H12C H 0.2957 -0.0983 0.0841 0.059 Uiso 1 1 calc R . . C134 C 0.42020(18) 0.0577(6) 0.10734(15) 0.0328(18) Uani 1 1 d . . . C135 C 0.4259(2) -0.0326(7) 0.13145(19) 0.059(2) Uani 1 1 d . . . H14I H 0.4051 -0.0765 0.1414 0.071 Uiso 1 1 calc R . . C136 C 0.4648(3) -0.0567(9) 0.14079(19) 0.079(3) Uani 1 1 d . . . H14H H 0.4704 -0.1158 0.1582 0.095 Uiso 1 1 calc R . . C137 C 0.4941(2) 0.0038(10) 0.1252(2) 0.084(3) Uani 1 1 d . . . H13I H 0.5199 -0.0146 0.1312 0.101 Uiso 1 1 calc R . . C138 C 0.4865(2) 0.0908(8) 0.1007(2) 0.074(3) Uani 1 1 d . . . H13G H 0.5070 0.1333 0.0898 0.089 Uiso 1 1 calc R . . C139 C 0.44883(19) 0.1173(7) 0.09180(18) 0.047(2) Uani 1 1 d . . . H13B H 0.4434 0.1776 0.0747 0.057 Uiso 1 1 calc R . . C140 C 0.35374(19) 0.2851(6) 0.17049(16) 0.0358(18) Uani 1 1 d . . . C141 C 0.3804(2) 0.3569(7) 0.18801(17) 0.052(2) Uani 1 1 d . . . H13C H 0.4071 0.3501 0.1833 0.063 Uiso 1 1 calc R . . C142 C 0.3666(3) 0.4387(7) 0.21262(19) 0.068(3) Uani 1 1 d . . . H13E H 0.3842 0.4893 0.2248 0.082 Uiso 1 1 calc R . . C143 C 0.3274(3) 0.4480(8) 0.21975(19) 0.066(3) Uani 1 1 d . . . H13D H 0.3183 0.5035 0.2370 0.079 Uiso 1 1 calc R . . C144 C 0.3021(2) 0.3768(7) 0.20183(19) 0.061(3) Uani 1 1 d . . . H13F H 0.2754 0.3854 0.2062 0.073 Uiso 1 1 calc R . . C145 C 0.3147(2) 0.2906(7) 0.17689(16) 0.046(2) Uani 1 1 d . . . H13H H 0.2972 0.2390 0.1651 0.056 Uiso 1 1 calc R . . C146 C 0.3481(2) 0.3828(7) -0.00926(17) 0.051(2) Uani 1 1 d . . . H14B H 0.3256 0.3654 -0.0244 0.061 Uiso 1 1 calc R . . H14C H 0.3693 0.4154 -0.0239 0.061 Uiso 1 1 calc R . . C147 C 0.41330(18) 0.2335(6) 0.00666(15) 0.0349(18) Uani 1 1 d . . . C148 C 0.43839(17) 0.3311(7) 0.00748(15) 0.0357(17) Uani 1 1 d . . . H15B H 0.4289 0.4097 0.0115 0.043 Uiso 1 1 calc R . . C149 C 0.4781(2) 0.3113(8) 0.00223(18) 0.060(2) Uani 1 1 d . . . H15D H 0.4953 0.3771 0.0032 0.072 Uiso 1 1 calc R . . C150 C 0.4918(2) 0.2005(8) -0.00411(17) 0.055(2) Uani 1 1 d . . . H15E H 0.5186 0.1893 -0.0074 0.066 Uiso 1 1 calc R . . C151 C 0.4674(2) 0.1030(7) -0.00589(17) 0.049(2) Uani 1 1 d . . . H15C H 0.4775 0.0257 -0.0110 0.059 Uiso 1 1 calc R . . C152 C 0.42816(19) 0.1180(7) -0.00021(16) 0.0407(19) Uani 1 1 d . . . H15F H 0.4114 0.0508 -0.0010 0.049 Uiso 1 1 calc R . . C153 C 0.33915(17) 0.1221(6) -0.00225(17) 0.0344(17) Uani 1 1 d . . . C154 C 0.3278(2) 0.0279(7) 0.01848(18) 0.051(2) Uani 1 1 d . . . H16B H 0.3313 0.0316 0.0435 0.061 Uiso 1 1 calc R . . C155 C 0.3116(2) -0.0713(8) 0.00356(17) 0.058(2) Uani 1 1 d . . . H16E H 0.3035 -0.1360 0.0182 0.069 Uiso 1 1 calc R . . C156 C 0.3068(2) -0.0776(7) -0.03413(17) 0.048(2) Uani 1 1 d . . . H16C H 0.2960 -0.1471 -0.0448 0.057 Uiso 1 1 calc R . . C157 C 0.31801(19) 0.0187(7) -0.05508(19) 0.054(2) Uani 1 1 d . . . H16I H 0.3141 0.0173 -0.0801 0.064 Uiso 1 1 calc R . . C158 C 0.33507(19) 0.1172(7) -0.03893(15) 0.045(2) Uani 1 1 d . . . H16H H 0.3440 0.1819 -0.0531 0.054 Uiso 1 1 calc R . . C159 C 0.29058(19) 0.5471(6) 0.01941(16) 0.0394(19) Uani 1 1 d . . . C160 C 0.26095(19) 0.5566(7) 0.04482(18) 0.050(2) Uani 1 1 d . . . H14D H 0.2652 0.5259 0.0680 0.061 Uiso 1 1 calc R . . C161 C 0.2267(2) 0.6081(7) 0.0372(2) 0.064(2) Uani 1 1 d . . . H146 H 0.2077 0.6115 0.0553 0.077 Uiso 1 1 calc R . . C162 C 0.2186(2) 0.6548(7) 0.0049(2) 0.057(2) Uani 1 1 d . . . H14J H 0.1946 0.6918 0.0000 0.068 Uiso 1 1 calc R . . C163 C 0.24705(19) 0.6457(7) -0.02057(19) 0.056(2) Uani 1 1 d . . . H14K H 0.2420 0.6741 -0.0439 0.067 Uiso 1 1 calc R . . C164 C 0.2822(2) 0.5973(7) -0.01336(17) 0.052(2) Uani 1 1 d . . . H14E H 0.3014 0.5981 -0.0313 0.062 Uiso 1 1 calc R . . C165 C 0.36809(19) 0.6044(6) 0.02808(15) 0.0379(18) Uani 1 1 d . . . C166 C 0.3859(2) 0.6551(7) -0.00173(18) 0.053(2) Uani 1 1 d . . . H16D H 0.3808 0.6201 -0.0242 0.064 Uiso 1 1 calc R . . C167 C 0.4100(2) 0.7508(7) -0.0007(2) 0.060(2) Uani 1 1 d . . . H16G H 0.4218 0.7799 -0.0218 0.072 Uiso 1 1 calc R . . C168 C 0.4168(2) 0.8039(7) 0.0309(2) 0.070(3) Uani 1 1 d . . . H16F H 0.4334 0.8714 0.0321 0.084 Uiso 1 1 calc R . . C169 C 0.3998(3) 0.7604(8) 0.06181(18) 0.077(3) Uani 1 1 d . . . H16J H 0.4053 0.7973 0.0840 0.093 Uiso 1 1 calc R . . C170 C 0.3756(2) 0.6668(7) 0.06063(18) 0.066(3) Uani 1 1 d . . . H15G H 0.3631 0.6415 0.0818 0.080 Uiso 1 1 calc R . . P5 P 0.09890(6) 0.6125(3) 0.01631(6) 0.0704(8) Uani 1 1 d . . . F1 F 0.09712(18) 0.7305(6) -0.00665(13) 0.122(2) Uani 1 1 d . . . F2 F 0.12865(13) 0.5576(6) -0.01097(12) 0.112(2) Uani 1 1 d . . . F3 F 0.13220(13) 0.6696(7) 0.03964(15) 0.139(3) Uani 1 1 d . . . F4 F 0.10114(19) 0.4980(6) 0.04011(15) 0.142(3) Uani 1 1 d . . . F5 F 0.06543(12) 0.5566(5) -0.00721(12) 0.0956(19) Uani 1 1 d . . . F6 F 0.06795(12) 0.6688(6) 0.04236(11) 0.0975(19) Uani 1 1 d . . . P105 P -0.16900(6) -0.6456(3) -0.11683(6) 0.0970(12) Uani 1 1 d . . . F101 F -0.12998(13) -0.6684(9) -0.13587(12) 0.192(4) Uani 1 1 d . . . F102 F -0.15081(19) -0.5858(15) -0.08504(15) 0.364(11) Uani 1 1 d . . . F103 F -0.18809(15) -0.6929(6) -0.15095(13) 0.116(2) Uani 1 1 d . . . F104 F -0.20812(13) -0.6403(7) -0.09814(12) 0.128(3) Uani 1 1 d . . . F105 F -0.1651(3) -0.7688(12) -0.1016(3) 0.396(12) Uani 1 1 d . . . F106 F -0.1721(3) -0.5255(8) -0.1343(2) 0.224(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn2 0.038 0.054 0.040 -0.001 0.003 0.012 Mn1 0.0300(6) 0.0352(7) 0.0290(5) 0.0028(5) -0.0007(5) -0.0006(6) P1 0.0330(11) 0.0324(12) 0.0342(10) 0.0030(9) -0.0019(9) -0.0006(9) P2 0.0315(11) 0.0347(12) 0.0317(10) 0.0024(9) -0.0006(9) -0.0011(9) P3 0.0354(11) 0.0366(12) 0.0299(10) 0.0024(10) -0.0020(8) -0.0028(10) P4 0.0358(12) 0.0728(19) 0.0383(12) 0.0023(12) 0.0020(10) 0.0066(12) O1 0.083(5) 0.088(5) 0.061(4) 0.013(4) 0.019(3) 0.006(4) O2 0.093(4) 0.053(4) 0.038(3) 0.001(3) -0.013(3) -0.029(3) O3 0.031(3) 0.077(4) 0.052(3) 0.001(3) 0.013(2) 0.012(3) O4 0.040(3) 0.069(4) 0.041(3) -0.013(3) -0.010(2) 0.007(3) O5 0.051(4) 0.109(5) 0.053(3) 0.008(4) 0.018(3) 0.011(4) O6 0.065(4) 0.058(4) 0.055(3) -0.001(3) -0.024(3) 0.024(3) O7 0.044(3) 0.034(3) 0.036(3) -0.001(2) -0.004(2) -0.004(3) O8 0.045(3) 0.050(3) 0.025(2) 0.001(2) 0.003(2) -0.001(3) O9 0.050(3) 0.049(3) 0.025(3) 0.005(2) -0.011(2) -0.010(3) N1 0.050(4) 0.043(4) 0.033(3) -0.002(3) -0.001(3) 0.005(4) N2 0.054(4) 0.071(6) 0.043(4) 0.010(4) 0.021(3) 0.017(4) C1 0.051(5) 0.022(4) 0.027(4) 0.002(3) -0.004(3) 0.005(4) C2 0.052(5) 0.030(5) 0.021(4) 0.016(3) 0.004(3) -0.008(4) C3 0.034(4) 0.041(5) 0.022(4) -0.001(3) -0.005(3) 0.017(4) C4 0.077(7) 0.091(8) 0.056(5) -0.008(5) 0.033(5) -0.001(6) C5 0.022(4) 0.067(7) 0.042(5) -0.012(4) 0.006(3) -0.005(5) C6 0.039(5) 0.113(9) 0.030(4) -0.010(5) -0.002(3) 0.009(6) C7 0.082(8) 0.045(6) 0.054(5) 0.008(5) 0.023(5) 0.020(6) C8 0.057(6) 0.097(9) 0.058(6) -0.037(6) 0.039(5) -0.021(6) C9 0.060(6) 0.080(8) 0.035(4) -0.017(5) 0.016(4) 0.007(5) C10 0.047(5) 0.073(7) 0.037(4) 0.017(5) -0.011(4) 0.018(6) C11 0.060(6) 0.070(7) 0.070(6) -0.014(6) -0.024(5) 0.038(6) C12 0.109(9) 0.102(10) 0.062(6) 0.012(6) -0.021(6) 0.044(8) C13 0.093(10) 0.177(16) 0.078(8) -0.041(10) -0.002(7) 0.078(11) C14 0.039(6) 0.115(10) 0.089(7) -0.011(8) 0.012(5) 0.001(7) C15 0.049(6) 0.146(11) 0.037(5) -0.031(6) -0.008(4) -0.012(7) C16 0.043(5) 0.106(9) 0.039(5) -0.006(6) 0.018(4) -0.001(6) C17 0.062(7) 0.119(10) 0.040(5) 0.004(6) 0.000(4) -0.004(7) C18 0.088(9) 0.149(12) 0.096(9) 0.056(9) 0.035(7) 0.049(8) C19 0.040(9) 0.52(4) 0.134(14) 0.19(2) 0.022(8) 0.039(14) C20 0.064(9) 0.58(4) 0.040(7) 0.049(13) -0.038(6) -0.094(14) C21 0.121(9) 0.251(15) 0.029(5) 0.022(7) -0.017(6) -0.134(10) C22 0.072(7) 0.057(6) 0.046(5) -0.013(5) -0.022(5) 0.018(6) C23 0.115(9) 0.047(7) 0.057(6) 0.005(5) -0.002(6) -0.006(6) C24 0.113(9) 0.105(10) 0.061(6) -0.012(7) -0.012(6) -0.023(8) C25 0.102(9) 0.088(9) 0.085(8) -0.029(7) -0.069(7) 0.014(8) C26 0.114(11) 0.110(11) 0.150(11) -0.061(9) -0.030(9) 0.038(9) C27 0.048(6) 0.117(10) 0.100(7) -0.053(7) -0.033(5) 0.040(6) C28 0.056(5) 0.026(5) 0.031(4) 0.008(4) -0.013(4) 0.017(4) C29 0.060(5) 0.035(5) 0.056(5) 0.022(4) 0.020(4) 0.004(4) C30 0.053(5) 0.063(7) 0.064(6) 0.013(5) 0.025(4) 0.011(5) C31 0.119(8) 0.035(6) 0.043(5) 0.008(4) 0.003(5) 0.003(6) C32 0.120(8) 0.046(6) 0.027(4) 0.005(4) -0.024(4) 0.013(6) C33 0.087(6) 0.054(6) 0.026(4) -0.020(4) -0.006(4) 0.004(5) C34 0.066(6) 0.035(5) 0.033(4) 0.001(4) -0.006(4) 0.000(4) C35 0.068(6) 0.048(6) 0.047(5) -0.003(4) -0.014(4) -0.010(5) C36 0.085(7) 0.057(6) 0.053(5) -0.003(5) -0.022(5) -0.006(5) C37 0.141(11) 0.096(10) 0.071(8) -0.003(7) -0.029(9) 0.003(10) C38 0.142(11) 0.076(9) 0.051(6) -0.019(6) 0.003(7) 0.021(9) C39 0.076(6) 0.080(8) 0.053(6) 0.011(5) 0.035(5) 0.015(6) C40 0.053(6) 0.066(7) 0.028(4) -0.014(4) -0.011(4) -0.007(5) C41 0.048(5) 0.069(7) 0.062(6) 0.000(5) -0.007(4) -0.011(5) C42 0.052(6) 0.097(9) 0.069(6) -0.027(6) 0.006(5) -0.038(7) C43 0.101(10) 0.104(10) 0.047(6) 0.007(6) -0.005(6) -0.067(9) C44 0.090(8) 0.087(8) 0.063(6) 0.045(6) -0.035(6) -0.055(8) C45 0.065(6) 0.052(6) 0.047(5) 0.020(5) -0.014(4) -0.029(5) C46 0.029(4) 0.033(5) 0.047(4) 0.007(4) 0.005(3) 0.009(4) C47 0.037(4) 0.051(6) 0.019(3) 0.001(3) -0.002(3) -0.001(4) C48 0.045(5) 0.077(7) 0.053(5) 0.017(5) 0.004(4) -0.029(5) C49 0.049(6) 0.072(7) 0.052(5) -0.013(5) -0.026(4) 0.015(5) C50 0.027(4) 0.071(7) 0.065(5) -0.015(5) -0.006(4) -0.001(5) C51 0.040(5) 0.073(7) 0.058(5) -0.010(5) 0.020(4) -0.014(5) C52 0.034(5) 0.047(5) 0.041(4) 0.006(4) -0.008(3) -0.004(4) C53 0.033(4) 0.033(5) 0.042(4) -0.001(4) 0.012(3) 0.003(4) C54 0.048(5) 0.071(7) 0.051(5) 0.008(5) -0.002(4) 0.005(5) C55 0.064(6) 0.066(7) 0.052(5) -0.028(5) 0.000(5) 0.018(5) C56 0.062(6) 0.058(7) 0.073(7) -0.027(6) 0.025(5) 0.004(5) C57 0.099(8) 0.040(6) 0.090(8) 0.013(6) 0.016(6) 0.020(6) C58 0.047(5) 0.046(5) 0.044(4) -0.018(4) -0.010(4) 0.018(4) C59 0.030(4) 0.056(5) 0.023(4) 0.000(4) -0.004(3) 0.007(4) C60 0.039(5) 0.066(6) 0.040(5) 0.005(4) 0.002(4) -0.004(4) C61 0.030(4) 0.062(6) 0.033(4) 0.017(4) 0.005(3) 0.010(4) C62 0.026(4) 0.051(6) 0.063(5) 0.004(4) 0.003(4) -0.016(4) C63 0.055(5) 0.057(6) 0.061(6) 0.010(5) 0.004(4) -0.006(5) C64 0.044(5) 0.053(6) 0.040(4) 0.018(4) 0.000(4) -0.018(4) C65 0.037(4) 0.034(5) 0.038(4) -0.010(4) -0.001(4) -0.017(4) C66 0.057(5) 0.045(6) 0.049(5) -0.001(4) -0.009(4) -0.001(4) C67 0.119(8) 0.078(8) 0.053(6) -0.020(6) -0.015(6) 0.014(7) C68 0.091(7) 0.047(6) 0.083(7) 0.000(6) -0.040(6) 0.031(5) C69 0.063(6) 0.063(7) 0.053(5) -0.004(5) -0.035(4) -0.008(5) C70 0.066(6) 0.043(5) 0.038(5) 0.003(4) -0.018(4) 0.013(5) Mn102 0.0400(6) 0.0564(8) 0.0269(5) -0.0044(6) -0.0040(5) -0.0024(6) Mn101 0.0365(6) 0.0385(7) 0.0257(5) -0.0023(6) -0.0014(5) -0.0010(6) P101 0.0286(10) 0.0425(13) 0.0233(9) -0.0033(9) -0.0002(8) -0.0024(10) P102 0.0368(11) 0.0370(12) 0.0251(9) 0.0015(9) -0.0041(8) 0.0001(10) P103 0.0390(11) 0.0375(12) 0.0272(10) -0.0061(9) -0.0054(8) -0.0010(10) P104 0.0398(13) 0.0884(19) 0.0297(10) -0.0070(11) 0.0001(9) -0.0079(13) O101 0.074 0.072 0.074 0.006 -0.030 -0.009 O102 0.084 0.039 0.030 -0.006 -0.002 0.014 O103 0.060 0.059 0.057 -0.011 -0.014 0.002 O104 0.040 0.183 0.027 -0.021 0.005 -0.031 O105 0.039 0.113 0.029 -0.001 -0.005 -0.006 O106 0.092 0.086 0.039 -0.012 -0.008 0.014 O107 0.046 0.044 0.026 0.012 -0.008 -0.015 O108 0.045 0.050 0.043 0.001 -0.012 0.010 O109 0.038 0.040 0.016 0.000 -0.007 0.005 N101 0.027(3) 0.059(5) 0.022(3) -0.003(3) 0.001(3) 0.012(3) N102 0.052(4) 0.057(5) 0.040(3) -0.003(3) -0.006(3) -0.004(3) C101 0.035(4) 0.031(5) 0.015(3) -0.002(3) 0.012(3) 0.012(4) C103 0.062(5) 0.028(5) 0.034(4) -0.006(3) -0.014(3) 0.008(4) C102 0.048(5) 0.029(5) 0.043(4) 0.007(4) -0.006(3) 0.005(4) C104 0.120(8) 0.111(10) 0.043(5) -0.022(6) -0.009(5) -0.029(7) C105 0.064(6) 0.080(7) 0.024(4) -0.008(5) -0.009(4) -0.006(6) C106 0.050(5) 0.111(9) 0.018(4) 0.006(5) 0.001(3) 0.014(6) C107 0.073(7) 0.085(9) 0.063(6) 0.026(6) -0.024(6) -0.010(7) C108 0.113(9) 0.082(9) 0.032(5) -0.018(5) -0.024(5) 0.038(7) C109 0.047(5) 0.132(10) 0.027(4) -0.009(6) -0.008(4) 0.017(6) C110 0.063(7) 0.126(11) 0.049(5) -0.020(6) 0.022(5) -0.028(7) C111 0.185(14) 0.097(11) 0.120(10) -0.029(8) 0.081(9) -0.067(10) C112 0.27(2) 0.199(18) 0.141(14) -0.101(13) 0.104(15) -0.146(19) C113 0.132(15) 0.39(3) 0.131(13) -0.114(18) 0.072(11) -0.164(18) C114 0.061(9) 0.51(4) 0.069(8) -0.075(14) 0.028(6) -0.071(14) C115 0.053(6) 0.225(15) 0.056(6) -0.030(8) 0.022(5) -0.004(9) C116 0.051(5) 0.118(9) 0.026(4) 0.001(5) 0.011(4) -0.018(6) C117 0.086(7) 0.097(9) 0.054(6) 0.029(6) 0.018(5) 0.027(7) C118 0.062(7) 0.141(11) 0.110(9) 0.052(9) 0.015(6) 0.033(7) C119 0.088(8) 0.234(18) 0.058(7) 0.078(9) 0.024(6) 0.026(10) C120 0.128(10) 0.207(16) 0.056(7) 0.010(8) 0.038(7) -0.064(11) C121 0.092(7) 0.121(10) 0.070(6) -0.021(7) 0.022(6) -0.052(7) C122 0.085(8) 0.118(10) 0.077(7) -0.055(6) -0.011(6) -0.009(7) C123 0.074(7) 0.119(9) 0.045(5) -0.013(6) 0.023(5) -0.028(6) C124 0.097(8) 0.117(10) 0.082(7) -0.046(7) -0.012(6) -0.014(7) C125 0.119(11) 0.34(2) 0.171(13) -0.172(15) 0.071(10) -0.046(13) C126 0.128(14) 0.72(5) 0.57(4) -0.57(4) 0.18(2) -0.20(2) C127 0.056(8) 0.33(2) 0.33(2) -0.298(18) 0.053(10) -0.039(10) C128 0.042(5) 0.025(5) 0.052(5) 0.007(4) -0.013(4) 0.004(4) C129 0.062(5) 0.056(6) 0.035(4) 0.004(4) -0.003(4) -0.018(5) C130 0.074(6) 0.034(5) 0.042(5) 0.016(4) 0.006(4) -0.009(5) C131 0.064(5) 0.046(6) 0.039(5) 0.014(4) 0.002(4) 0.005(5) C132 0.098(7) 0.031(5) 0.048(5) -0.013(4) 0.015(5) -0.011(5) C133 0.053(5) 0.047(6) 0.048(5) 0.008(5) 0.005(4) -0.003(4) C134 0.036(4) 0.049(5) 0.014(3) -0.002(3) 0.006(3) 0.021(4) C135 0.069(6) 0.059(6) 0.050(5) -0.011(5) 0.005(4) 0.020(5) C136 0.113(9) 0.093(9) 0.031(5) -0.021(5) -0.006(6) 0.055(7) C137 0.059(7) 0.153(11) 0.040(5) -0.018(6) -0.015(5) 0.032(7) C138 0.053(6) 0.107(9) 0.063(6) 0.001(6) -0.008(5) 0.009(6) C139 0.038(5) 0.058(6) 0.046(5) -0.002(4) -0.011(4) 0.018(4) C140 0.043(5) 0.031(5) 0.034(4) 0.001(3) -0.002(3) 0.012(4) C141 0.058(5) 0.052(6) 0.046(5) -0.008(4) -0.006(4) -0.012(5) C142 0.111(8) 0.046(6) 0.048(5) -0.011(5) -0.010(5) -0.006(6) C143 0.099(8) 0.051(7) 0.048(5) -0.002(5) 0.008(6) 0.036(6) C144 0.069(6) 0.061(7) 0.051(5) 0.020(5) 0.008(5) 0.030(5) C145 0.055(5) 0.064(6) 0.020(4) 0.002(4) 0.014(3) 0.013(5) C146 0.055(5) 0.064(6) 0.033(4) 0.000(4) -0.007(4) 0.008(4) C147 0.033(4) 0.049(5) 0.023(4) -0.002(3) 0.004(3) 0.011(4) C148 0.029(4) 0.048(5) 0.030(4) 0.002(4) 0.002(3) -0.019(4) C149 0.035(5) 0.090(8) 0.055(5) 0.016(5) -0.004(4) -0.023(5) C150 0.030(5) 0.095(8) 0.039(5) 0.002(5) -0.008(4) 0.002(6) C151 0.047(5) 0.060(6) 0.041(5) -0.007(4) -0.004(4) 0.019(5) C152 0.043(5) 0.049(5) 0.030(4) 0.012(4) 0.004(3) 0.004(4) C153 0.023(4) 0.038(5) 0.042(4) -0.007(4) 0.012(3) -0.002(3) C154 0.068(6) 0.048(6) 0.038(4) 0.006(4) -0.009(4) -0.018(5) C155 0.084(6) 0.063(6) 0.026(4) -0.013(4) 0.012(4) -0.028(5) C156 0.070(6) 0.037(5) 0.037(4) -0.013(4) 0.004(4) -0.034(4) C157 0.050(5) 0.066(6) 0.044(5) -0.029(5) 0.001(4) -0.019(5) C158 0.059(5) 0.059(6) 0.017(4) -0.003(4) 0.000(3) -0.013(4) C159 0.044(5) 0.042(5) 0.032(4) 0.017(4) -0.006(4) 0.008(4) C160 0.045(5) 0.065(6) 0.041(5) 0.003(4) 0.000(4) 0.015(5) C161 0.059(6) 0.073(7) 0.060(6) 0.014(5) 0.004(5) 0.031(5) C162 0.033(5) 0.042(6) 0.094(6) 0.026(5) -0.008(5) 0.011(4) C163 0.029(5) 0.082(7) 0.056(5) 0.020(5) -0.011(4) 0.006(5) C164 0.064(6) 0.058(6) 0.033(4) 0.008(4) 0.004(4) 0.000(5) C165 0.054(5) 0.042(5) 0.018(4) -0.006(3) -0.002(3) -0.008(4) C166 0.068(6) 0.055(6) 0.038(4) -0.003(4) -0.002(4) -0.010(5) C167 0.066(6) 0.040(6) 0.074(6) -0.015(5) 0.017(5) -0.019(5) C168 0.076(6) 0.029(5) 0.104(7) 0.025(6) -0.010(6) -0.015(5) C169 0.135(9) 0.067(7) 0.029(4) -0.003(4) -0.011(5) -0.060(7) C170 0.113(7) 0.046(6) 0.040(5) 0.003(4) 0.025(5) -0.011(6) P5 0.0478(15) 0.116(3) 0.0478(14) -0.0128(16) -0.0064(12) 0.0157(15) F1 0.164(6) 0.127(6) 0.074(4) 0.016(4) -0.001(4) -0.008(5) F2 0.054(3) 0.194(7) 0.089(4) -0.051(4) 0.008(3) 0.018(4) F3 0.061(3) 0.248(8) 0.107(4) -0.079(5) -0.018(3) 0.024(5) F4 0.181(7) 0.139(6) 0.107(5) 0.053(5) -0.022(4) 0.033(5) F5 0.054(3) 0.160(6) 0.073(3) -0.031(3) 0.002(3) -0.002(3) F6 0.063(3) 0.176(6) 0.053(3) -0.014(3) 0.005(2) 0.036(4) P105 0.0462(16) 0.201(4) 0.0439(15) 0.037(2) -0.0049(12) -0.023(2) F101 0.047(3) 0.468(14) 0.061(3) 0.077(6) 0.012(3) 0.010(6) F102 0.092(5) 0.95(3) 0.048(4) -0.059(10) -0.021(4) -0.138(12) F103 0.117(5) 0.139(6) 0.091(4) -0.036(4) 0.012(4) -0.047(4) F104 0.054(3) 0.252(8) 0.079(4) -0.041(4) 0.017(3) -0.045(4) F105 0.328(15) 0.428(19) 0.431(18) 0.379(17) 0.281(14) 0.284(15) F106 0.361(14) 0.143(8) 0.169(8) -0.055(7) 0.129(8) -0.083(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn2 N2 1.612(8) . ? Mn2 N1 1.927(6) . ? Mn2 C6 2.116(7) . ? Mn2 C9 2.133(7) . ? Mn2 C8 2.143(8) . ? Mn2 C5 2.144(7) . ? Mn2 C7 2.156(8) . ? Mn2 P4 2.218(2) . ? Mn1 C2 1.795(8) . ? Mn1 C3 1.798(7) . ? Mn1 C1 1.960(8) . ? Mn1 P3 2.197(2) . ? Mn1 P2 2.293(2) . ? Mn1 P1 2.324(2) . ? P1 C53 1.789(7) . ? P1 C47 1.813(7) . ? P1 C46 1.814(7) . ? P2 C65 1.784(7) . ? P2 C59 1.798(7) . ? P2 C46 1.802(7) . ? P3 O9 1.587(5) . ? P3 O7 1.599(5) . ? P3 O8 1.620(4) . ? P4 O6 1.572(6) . ? P4 O5 1.602(5) . ? P4 O4 1.608(5) . ? O1 N2 1.210(8) . ? O2 C2 1.133(7) . ? O3 C3 1.154(7) . ? O4 C10 1.427(9) . ? O5 C16 1.408(10) . ? O6 C22 1.432(9) . ? O7 C28 1.433(8) . ? O8 C34 1.423(8) . ? O9 C40 1.447(9) . ? N1 C1 1.180(7) . ? C4 C5 1.485(11) . ? C5 C9 1.408(10) . ? C5 C6 1.425(11) . ? C6 C7 1.374(11) . ? C7 C8 1.357(11) . ? C8 C9 1.412(11) . ? C10 C15 1.314(10) . ? C10 C11 1.357(11) . ? C11 C12 1.361(12) . ? C12 C13 1.360(14) . ? C13 C14 1.353(15) . ? C14 C15 1.390(13) . ? C16 C17 1.311(12) . ? C16 C21 1.358(11) . ? C17 C18 1.395(13) . ? C18 C19 1.32(2) . ? C19 C20 1.32(3) . ? C20 C21 1.45(2) . ? C22 C23 1.334(11) . ? C22 C27 1.400(11) . ? C23 C24 1.378(12) . ? C24 C25 1.357(13) . ? C25 C26 1.406(14) . ? C26 C27 1.442(13) . ? C28 C29 1.385(9) . ? C28 C33 1.392(9) . ? C29 C30 1.369(10) . ? C30 C31 1.385(9) . ? C31 C32 1.358(10) . ? C32 C33 1.376(10) . ? C34 C35 1.365(9) . ? C34 C39 1.393(9) . ? C35 C36 1.405(10) . ? C36 C37 1.446(13) . ? C37 C38 1.265(13) . ? C38 C39 1.393(12) . ? C40 C45 1.330(10) . ? C40 C41 1.341(10) . ? C41 C42 1.447(11) . ? C42 C43 1.316(13) . ? C43 C44 1.363(13) . ? C44 C45 1.370(10) . ? C47 C52 1.391(9) . ? C47 C48 1.415(10) . ? C48 C49 1.379(10) . ? C49 C50 1.375(10) . ? C50 C51 1.361(10) . ? C51 C52 1.379(9) . ? C53 C58 1.398(9) . ? C53 C54 1.420(9) . ? C54 C55 1.364(10) . ? C55 C56 1.350(11) . ? C56 C57 1.343(10) . ? C57 C58 1.369(10) . ? C59 C60 1.398(8) . ? C59 C64 1.412(8) . ? C60 C61 1.402(9) . ? C61 C62 1.373(9) . ? C62 C63 1.387(9) . ? C63 C64 1.413(9) . ? C65 C70 1.383(9) . ? C65 C66 1.386(9) . ? C66 C67 1.409(11) . ? C67 C68 1.370(10) . ? C68 C69 1.358(10) . ? C69 C70 1.372(10) . ? Mn102 N102 1.631(7) . ? Mn102 N101 1.935(6) . ? Mn102 C108 2.134(8) . ? Mn102 C109 2.137(7) . ? Mn102 C105 2.138(7) . ? Mn102 C106 2.157(6) . ? Mn102 C107 2.174(8) . ? Mn102 P104 2.204(2) . ? Mn101 C102 1.785(7) . ? Mn101 C103 1.814(7) . ? Mn101 C101 1.994(7) . ? Mn101 P103 2.208(2) . ? Mn101 P102 2.285(2) . ? Mn101 P101 2.348(2) . ? P101 C147 1.811(6) . ? P101 C146 1.837(7) . ? P101 C153 1.840(7) . ? P102 C165 1.775(7) . ? P102 C159 1.792(7) . ? P102 C146 1.857(7) . ? P103 O107 1.589(4) . ? P103 O108 1.625(5) . ? P103 O109 1.635(4) . ? P104 O104 1.585(5) . ? P104 O106 1.601(6) . ? P104 O105 1.618(5) . ? O101 N102 1.192(7) . ? O102 C102 1.170(7) . ? O103 C103 1.161(7) . ? O104 C110 1.328(6) . ? O105 C116 1.365(6) . ? O106 C122 1.363(6) . ? O107 C128 1.402(7) . ? O108 C134 1.412(7) . ? O109 C140 1.394(7) . ? N101 C101 1.147(7) . ? C104 C105 1.490(11) . ? C105 C109 1.421(11) . ? C105 C106 1.425(11) . ? C106 C107 1.412(12) . ? C107 C108 1.362(11) . ? C108 C109 1.460(12) . ? C110 C111 1.3900 . ? C110 C115 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C116 C117 1.3900 . ? C116 C121 1.3900 . ? C117 C118 1.3900 . ? C118 C119 1.3900 . ? C119 C120 1.3900 . ? C120 C121 1.3900 . ? C122 C123 1.3900 . ? C122 C127 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? C126 C127 1.3900 . ? C128 C133 1.376(9) . ? C128 C129 1.381(9) . ? C129 C130 1.358(9) . ? C130 C131 1.341(10) . ? C131 C132 1.357(9) . ? C132 C133 1.391(10) . ? C134 C139 1.333(9) . ? C134 C135 1.370(9) . ? C135 C136 1.427(11) . ? C136 C137 1.357(12) . ? C137 C138 1.364(12) . ? C138 C139 1.385(9) . ? C140 C145 1.382(9) . ? C140 C141 1.392(9) . ? C141 C142 1.386(10) . ? C142 C143 1.397(11) . ? C143 C144 1.364(11) . ? C144 C145 1.413(10) . ? C147 C148 1.397(9) . ? C147 C152 1.413(9) . ? C148 C149 1.414(9) . ? C149 C150 1.347(11) . ? C150 C151 1.381(10) . ? C151 C152 1.395(9) . ? C153 C154 1.368(9) . ? C153 C158 1.389(8) . ? C154 C155 1.363(9) . ? C155 C156 1.430(9) . ? C156 C157 1.389(10) . ? C157 C158 1.390(9) . ? C159 C164 1.386(8) . ? C159 C160 1.411(8) . ? C160 C161 1.353(9) . ? C161 C162 1.354(10) . ? C162 C163 1.383(10) . ? C163 C164 1.364(9) . ? C165 C166 1.401(9) . ? C165 C170 1.433(9) . ? C166 C167 1.359(10) . ? C167 C168 1.351(10) . ? C168 C169 1.392(10) . ? C169 C170 1.343(10) . ? P5 F4 1.562(6) . ? P5 F1 1.576(6) . ? P5 F2 1.582(5) . ? P5 F6 1.587(5) . ? P5 F3 1.588(5) . ? P5 F5 1.591(5) . ? P105 F105 1.496(10) . ? P105 F106 1.496(10) . ? P105 F102 1.509(8) . ? P105 F104 1.534(5) . ? P105 F103 1.539(6) . ? P105 F101 1.557(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn2 N1 98.9(3) . . ? N2 Mn2 C6 116.7(4) . . ? N1 Mn2 C6 91.9(3) . . ? N2 Mn2 C9 103.1(3) . . ? N1 Mn2 C9 152.6(3) . . ? C6 Mn2 C9 63.7(3) . . ? N2 Mn2 C8 140.5(4) . . ? N1 Mn2 C8 120.5(4) . . ? C6 Mn2 C8 62.7(3) . . ? C9 Mn2 C8 38.6(3) . . ? N2 Mn2 C5 90.5(3) . . ? N1 Mn2 C5 126.2(3) . . ? C6 Mn2 C5 39.1(3) . . ? C9 Mn2 C5 38.4(3) . . ? C8 Mn2 C5 64.5(3) . . ? N2 Mn2 C7 153.4(3) . . ? N1 Mn2 C7 90.0(3) . . ? C6 Mn2 C7 37.5(3) . . ? C9 Mn2 C7 63.2(3) . . ? C8 Mn2 C7 36.8(3) . . ? C5 Mn2 C7 64.4(3) . . ? N2 Mn2 P4 98.6(2) . . ? N1 Mn2 P4 86.06(17) . . ? C6 Mn2 P4 144.4(3) . . ? C9 Mn2 P4 106.4(2) . . ? C8 Mn2 P4 88.0(2) . . ? C5 Mn2 P4 144.7(2) . . ? C7 Mn2 P4 106.9(3) . . ? C2 Mn1 C3 89.7(3) . . ? C2 Mn1 C1 90.0(3) . . ? C3 Mn1 C1 178.7(3) . . ? C2 Mn1 P3 97.0(2) . . ? C3 Mn1 P3 87.8(2) . . ? C1 Mn1 P3 90.93(19) . . ? C2 Mn1 P2 95.6(2) . . ? C3 Mn1 P2 94.9(2) . . ? C1 Mn1 P2 86.38(19) . . ? P3 Mn1 P2 167.05(8) . . ? C2 Mn1 P1 168.0(2) . . ? C3 Mn1 P1 92.1(2) . . ? C1 Mn1 P1 88.45(19) . . ? P3 Mn1 P1 94.94(8) . . ? P2 Mn1 P1 72.35(7) . . ? C53 P1 C47 102.3(3) . . ? C53 P1 C46 104.7(3) . . ? C47 P1 C46 107.7(3) . . ? C53 P1 Mn1 128.6(2) . . ? C47 P1 Mn1 117.2(2) . . ? C46 P1 Mn1 93.6(2) . . ? C65 P2 C59 102.9(3) . . ? C65 P2 C46 105.9(3) . . ? C59 P2 C46 106.5(3) . . ? C65 P2 Mn1 121.8(2) . . ? C59 P2 Mn1 122.4(2) . . ? C46 P2 Mn1 95.0(2) . . ? O9 P3 O7 104.2(3) . . ? O9 P3 O8 97.4(2) . . ? O7 P3 O8 104.2(2) . . ? O9 P3 Mn1 112.42(17) . . ? O7 P3 Mn1 115.18(18) . . ? O8 P3 Mn1 120.9(2) . . ? O6 P4 O5 102.5(3) . . ? O6 P4 O4 103.3(3) . . ? O5 P4 O4 99.8(3) . . ? O6 P4 Mn2 110.5(2) . . ? O5 P4 Mn2 118.4(2) . . ? O4 P4 Mn2 120.1(2) . . ? C10 O4 P4 124.1(5) . . ? C16 O5 P4 126.1(5) . . ? C22 O6 P4 124.6(5) . . ? C28 O7 P3 125.8(4) . . ? C34 O8 P3 124.1(4) . . ? C40 O9 P3 130.8(4) . . ? C1 N1 Mn2 173.4(6) . . ? O1 N2 Mn2 171.1(6) . . ? N1 C1 Mn1 178.7(6) . . ? O2 C2 Mn1 177.9(7) . . ? O3 C3 Mn1 175.6(5) . . ? C9 C5 C6 104.6(8) . . ? C9 C5 C4 126.9(8) . . ? C6 C5 C4 128.4(8) . . ? C9 C5 Mn2 70.4(4) . . ? C6 C5 Mn2 69.4(4) . . ? C4 C5 Mn2 126.8(5) . . ? C7 C6 C5 109.9(7) . . ? C7 C6 Mn2 72.8(4) . . ? C5 C6 Mn2 71.5(4) . . ? C8 C7 C6 108.5(8) . . ? C8 C7 Mn2 71.1(5) . . ? C6 C7 Mn2 69.7(5) . . ? C7 C8 C9 108.5(8) . . ? C7 C8 Mn2 72.1(5) . . ? C9 C8 Mn2 70.4(5) . . ? C5 C9 C8 108.5(8) . . ? C5 C9 Mn2 71.2(4) . . ? C8 C9 Mn2 71.1(4) . . ? C15 C10 C11 123.3(10) . . ? C15 C10 O4 119.1(10) . . ? C11 C10 O4 117.7(8) . . ? C10 C11 C12 118.7(10) . . ? C13 C12 C11 118.2(12) . . ? C14 C13 C12 122.9(12) . . ? C13 C14 C15 117.3(10) . . ? C10 C15 C14 119.4(11) . . ? C17 C16 C21 122.8(10) . . ? C17 C16 O5 120.5(8) . . ? C21 C16 O5 116.5(10) . . ? C16 C17 C18 123.5(10) . . ? C19 C18 C17 117.0(15) . . ? C18 C19 C20 119.6(15) . . ? C19 C20 C21 125.8(12) . . ? C16 C21 C20 111.1(11) . . ? C23 C22 C27 123.3(9) . . ? C23 C22 O6 118.5(8) . . ? C27 C22 O6 117.6(9) . . ? C22 C23 C24 119.1(10) . . ? C25 C24 C23 122.8(11) . . ? C24 C25 C26 118.4(10) . . ? C25 C26 C27 119.8(11) . . ? C22 C27 C26 116.1(9) . . ? C29 C28 C33 120.9(7) . . ? C29 C28 O7 115.6(6) . . ? C33 C28 O7 123.5(7) . . ? C30 C29 C28 117.9(7) . . ? C29 C30 C31 123.1(8) . . ? C32 C31 C30 116.7(8) . . ? C31 C32 C33 123.5(8) . . ? C32 C33 C28 117.8(7) . . ? C35 C34 C39 121.6(8) . . ? C35 C34 O8 124.3(7) . . ? C39 C34 O8 114.0(7) . . ? C34 C35 C36 119.7(8) . . ? C35 C36 C37 116.0(9) . . ? C38 C37 C36 122.7(11) . . ? C37 C38 C39 122.3(11) . . ? C34 C39 C38 117.6(9) . . ? C45 C40 C41 122.9(9) . . ? C45 C40 O9 120.0(8) . . ? C41 C40 O9 116.6(8) . . ? C40 C41 C42 118.1(9) . . ? C43 C42 C41 117.2(10) . . ? C42 C43 C44 123.3(10) . . ? C43 C44 C45 119.0(10) . . ? C40 C45 C44 119.3(9) . . ? P2 C46 P1 97.8(3) . . ? C52 C47 C48 118.5(6) . . ? C52 C47 P1 121.0(6) . . ? C48 C47 P1 120.0(6) . . ? C49 C48 C47 119.4(8) . . ? C50 C49 C48 121.5(8) . . ? C51 C50 C49 118.7(7) . . ? C50 C51 C52 122.1(8) . . ? C51 C52 C47 119.7(7) . . ? C58 C53 C54 116.9(7) . . ? C58 C53 P1 122.1(5) . . ? C54 C53 P1 121.0(6) . . ? C55 C54 C53 120.3(7) . . ? C56 C55 C54 121.3(8) . . ? C57 C56 C55 119.3(8) . . ? C56 C57 C58 122.6(9) . . ? C57 C58 C53 119.5(7) . . ? C60 C59 C64 117.6(6) . . ? C60 C59 P2 122.1(5) . . ? C64 C59 P2 120.2(5) . . ? C59 C60 C61 121.3(7) . . ? C62 C61 C60 119.8(6) . . ? C61 C62 C63 121.4(7) . . ? C62 C63 C64 118.6(7) . . ? C59 C64 C63 121.2(6) . . ? C70 C65 C66 114.9(7) . . ? C70 C65 P2 124.2(6) . . ? C66 C65 P2 120.7(6) . . ? C65 C66 C67 121.6(7) . . ? C68 C67 C66 119.5(8) . . ? C69 C68 C67 120.4(8) . . ? C68 C69 C70 118.6(7) . . ? C69 C70 C65 124.7(7) . . ? N102 Mn102 N101 100.6(3) . . ? N102 Mn102 C108 148.1(4) . . ? N101 Mn102 C108 110.9(4) . . ? N102 Mn102 C109 108.1(4) . . ? N101 Mn102 C109 149.7(3) . . ? C108 Mn102 C109 40.0(3) . . ? N102 Mn102 C105 89.7(3) . . ? N101 Mn102 C105 134.3(3) . . ? C108 Mn102 C105 64.6(3) . . ? C109 Mn102 C105 38.8(3) . . ? N102 Mn102 C106 108.6(4) . . ? N101 Mn102 C106 96.6(3) . . ? C108 Mn102 C106 63.6(3) . . ? C109 Mn102 C106 65.3(3) . . ? C105 Mn102 C106 38.8(3) . . ? N102 Mn102 C107 146.6(4) . . ? N101 Mn102 C107 85.9(3) . . ? C108 Mn102 C107 36.8(3) . . ? C109 Mn102 C107 64.7(3) . . ? C105 Mn102 C107 64.0(3) . . ? C106 Mn102 C107 38.1(3) . . ? N102 Mn102 P104 95.0(2) . . ? N101 Mn102 P104 86.16(15) . . ? C108 Mn102 P104 92.4(2) . . ? C109 Mn102 P104 100.7(2) . . ? C105 Mn102 P104 137.6(2) . . ? C106 Mn102 P104 155.2(3) . . ? C107 Mn102 P104 118.2(3) . . ? C102 Mn101 C103 88.3(3) . . ? C102 Mn101 C101 93.0(3) . . ? C103 Mn101 C101 177.5(3) . . ? C102 Mn101 P103 96.1(2) . . ? C103 Mn101 P103 88.5(2) . . ? C101 Mn101 P103 89.24(18) . . ? C102 Mn101 P102 92.0(2) . . ? C103 Mn101 P102 94.5(2) . . ? C101 Mn101 P102 87.54(18) . . ? P103 Mn101 P102 171.48(8) . . ? C102 Mn101 P101 164.3(2) . . ? C103 Mn101 P101 94.9(2) . . ? C101 Mn101 P101 84.44(16) . . ? P103 Mn101 P101 99.42(8) . . ? P102 Mn101 P101 72.41(7) . . ? C147 P101 C146 104.1(3) . . ? C147 P101 C153 104.4(3) . . ? C146 P101 C153 106.1(3) . . ? C147 P101 Mn101 121.2(2) . . ? C146 P101 Mn101 94.9(2) . . ? C153 P101 Mn101 122.9(2) . . ? C165 P102 C159 103.0(3) . . ? C165 P102 C146 107.4(3) . . ? C159 P102 C146 106.4(3) . . ? C165 P102 Mn101 119.1(2) . . ? C159 P102 Mn101 122.8(2) . . ? C146 P102 Mn101 96.4(2) . . ? O107 P103 O108 101.2(3) . . ? O107 P103 O109 103.5(2) . . ? O108 P103 O109 97.1(2) . . ? O107 P103 Mn101 114.69(18) . . ? O108 P103 Mn101 118.79(18) . . ? O109 P103 Mn101 118.50(18) . . ? O104 P104 O106 104.1(3) . . ? O104 P104 O105 99.8(3) . . ? O106 P104 O105 101.6(3) . . ? O104 P104 Mn102 122.2(2) . . ? O106 P104 Mn102 111.1(2) . . ? O105 P104 Mn102 115.5(2) . . ? C110 O104 P104 124.6(4) . . ? C116 O105 P104 127.6(4) . . ? C122 O106 P104 123.6(5) . . ? C128 O107 P103 126.9(4) . . ? C134 O108 P103 128.6(4) . . ? C140 O109 P103 123.7(4) . . ? C101 N101 Mn102 176.7(6) . . ? O101 N102 Mn102 173.7(6) . . ? N101 C101 Mn101 179.0(6) . . ? O103 C103 Mn101 178.1(6) . . ? O102 C102 Mn101 174.2(6) . . ? C109 C105 C106 109.0(8) . . ? C109 C105 C104 125.7(9) . . ? C106 C105 C104 125.2(9) . . ? C109 C105 Mn102 70.5(4) . . ? C106 C105 Mn102 71.4(4) . . ? C104 C105 Mn102 127.5(6) . . ? C107 C106 C105 107.2(8) . . ? C107 C106 Mn102 71.6(4) . . ? C105 C106 Mn102 69.9(4) . . ? C108 C107 C106 109.2(9) . . ? C108 C107 Mn102 70.0(5) . . ? C106 C107 Mn102 70.3(5) . . ? C107 C108 C109 109.6(9) . . ? C107 C108 Mn102 73.2(5) . . ? C109 C108 Mn102 70.1(5) . . ? C105 C109 C108 104.9(8) . . ? C105 C109 Mn102 70.6(4) . . ? C108 C109 Mn102 69.9(5) . . ? O104 C110 C111 119.0(8) . . ? O104 C110 C115 120.9(8) . . ? C111 C110 C115 120.0 . . ? C112 C111 C110 120.0 . . ? C111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C110 120.0 . . ? O105 C116 C117 122.4(5) . . ? O105 C116 C121 117.6(5) . . ? C117 C116 C121 120.0 . . ? C118 C117 C116 120.0 . . ? C117 C118 C119 120.0 . . ? C120 C119 C118 120.0 . . ? C119 C120 C121 120.0 . . ? C120 C121 C116 120.0 . . ? O106 C122 C123 121.6(5) . . ? O106 C122 C127 118.3(5) . . ? C123 C122 C127 120.0 . . ? C122 C123 C124 120.0 . . ? C125 C124 C123 120.0 . . ? C124 C125 C126 120.0 . . ? C125 C126 C127 120.0 . . ? C126 C127 C122 120.0 . . ? C133 C128 C129 120.1(7) . . ? C133 C128 O107 118.5(6) . . ? C129 C128 O107 121.0(6) . . ? C130 C129 C128 119.9(7) . . ? C131 C130 C129 120.6(7) . . ? C130 C131 C132 120.7(8) . . ? C131 C132 C133 120.5(8) . . ? C128 C133 C132 118.1(7) . . ? C139 C134 C135 123.3(7) . . ? C139 C134 O108 118.3(6) . . ? C135 C134 O108 117.8(7) . . ? C134 C135 C136 116.0(8) . . ? C137 C136 C135 120.9(9) . . ? C136 C137 C138 120.0(9) . . ? C137 C138 C139 120.0(9) . . ? C134 C139 C138 119.7(8) . . ? C145 C140 C141 123.2(7) . . ? C145 C140 O109 120.4(6) . . ? C141 C140 O109 116.4(6) . . ? C142 C141 C140 117.8(8) . . ? C141 C142 C143 121.0(9) . . ? C144 C143 C142 119.5(8) . . ? C143 C144 C145 121.6(8) . . ? C140 C145 C144 116.8(8) . . ? P101 C146 P102 95.6(3) . . ? C148 C147 C152 119.1(6) . . ? C148 C147 P101 120.3(6) . . ? C152 C147 P101 120.4(6) . . ? C147 C148 C149 119.1(7) . . ? C150 C149 C148 121.0(8) . . ? C149 C150 C151 120.9(8) . . ? C150 C151 C152 120.0(8) . . ? C151 C152 C147 119.8(7) . . ? C154 C153 C158 120.5(7) . . ? C154 C153 P101 120.8(5) . . ? C158 C153 P101 118.6(5) . . ? C155 C154 C153 120.6(7) . . ? C154 C155 C156 119.8(7) . . ? C157 C156 C155 119.5(7) . . ? C156 C157 C158 119.0(7) . . ? C153 C158 C157 120.6(7) . . ? C164 C159 C160 114.7(6) . . ? C164 C159 P102 122.5(5) . . ? C160 C159 P102 122.7(5) . . ? C161 C160 C159 122.2(7) . . ? C160 C161 C162 122.6(8) . . ? C161 C162 C163 116.3(7) . . ? C164 C163 C162 122.3(7) . . ? C163 C164 C159 121.8(7) . . ? C166 C165 C170 114.0(7) . . ? C166 C165 P102 127.6(5) . . ? C170 C165 P102 118.2(5) . . ? C167 C166 C165 124.7(7) . . ? C168 C167 C166 118.5(8) . . ? C167 C168 C169 120.5(8) . . ? C170 C169 C168 120.7(7) . . ? C169 C170 C165 121.4(7) . . ? F4 P5 F1 178.1(4) . . ? F4 P5 F2 91.3(4) . . ? F1 P5 F2 89.6(4) . . ? F4 P5 F6 90.2(3) . . ? F1 P5 F6 88.9(3) . . ? F2 P5 F6 177.7(3) . . ? F4 P5 F3 88.6(4) . . ? F1 P5 F3 89.8(4) . . ? F2 P5 F3 92.1(3) . . ? F6 P5 F3 89.7(3) . . ? F4 P5 F5 92.0(4) . . ? F1 P5 F5 89.7(3) . . ? F2 P5 F5 88.1(3) . . ? F6 P5 F5 90.1(3) . . ? F3 P5 F5 179.4(5) . . ? F105 P105 F106 176.4(7) . . ? F105 P105 F102 93.7(8) . . ? F106 P105 F102 88.9(8) . . ? F105 P105 F104 86.6(4) . . ? F106 P105 F104 95.9(5) . . ? F102 P105 F104 89.6(4) . . ? F105 P105 F103 92.5(8) . . ? F106 P105 F103 84.9(4) . . ? F102 P105 F103 173.8(8) . . ? F104 P105 F103 90.7(3) . . ? F105 P105 F101 87.0(5) . . ? F106 P105 F101 90.4(5) . . ? F102 P105 F101 94.0(4) . . ? F104 P105 F101 172.8(6) . . ? F103 P105 F101 86.4(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.351 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.064 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 1 0.048 0.531 0.099 263.5 48.0 2 -0.048 0.469 0.599 263.4 47.8 3 0.251 0.470 0.325 243.2 52.4 4 0.249 0.470 0.825 243.1 52.4 5 0.452 0.531 0.599 263.4 47.7 6 0.548 0.469 0.099 263.4 46.9 7 0.751 0.530 0.325 243.2 52.4 8 0.749 0.530 0.825 243.2 52.3 _platon_squeeze_details ; ;