Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global #=========================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof N. G. Connelly' _publ_contact_author_address ; Prof N. G. Connelly, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. UNITED KINGDOM ; _publ_contact_author_phone '0117 928 8162' _publ_contact_author_fax '0117 929 0509' _publ_contact_author_email 'Neil.Connelly@bris.ac.uk' _journal_coden_Cambridge 182 _publ_requested_journal 'J. Chem. Soc., Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Control over directional metal-metal charge transfer in cyanide-bridged dimanganese complexes: effects of m-CN linkage isomerism and ancillary ligands ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Anderson, Kirsty M.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Connelly, Neil G.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Llamas-Rey, Estefania' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Paul, Rowena L.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; #========================================================================== # 4. TEXT # # # N. G. CONNELLY # data_1+ _database_code_CSD 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_CSD 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