Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_mn1245s _database_code_CSD 175724 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Reger, Daniel' _publ_contact_author_name 'Dr Daniel Reger' _publ_contact_author_address ; Chemistry and Biochemistry University of South Carolina 631 Sumter Street, GSRC Columbia SC 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email 'REGER@MAIL.CHEM.SC.EDU' _publ_section_title ; Crystal Engineering Based on Tetrametallic Organometallic Building Blocks: Simultaneous Utilization of Intramolecular ð-ð stacking and Intermolecular Weak C-H···F Hydrogen Bonds ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; {C54H54N24O4[Mn(CO)3]4} {BF4}4 (CH3CN)6 (Et2O)2 ; _chemical_formula_sum 'C86 H92 B4 F16 Mn4 N30 O18' _chemical_formula_weight 2400.90 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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8441(9) _cell_length_b 17.6246(13) _cell_length_c 25.6874(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.538(2) _cell_angle_gamma 90.00 _cell_volume 5288.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6214 _cell_measurement_theta_min 2.311 _cell_measurement_theta_max 26.310 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7920 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 34997 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.40 _reflns_number_total 10830 _reflns_number_gt 7517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.619 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.1418P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10830 _refine_ls_number_parameters 712 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2164 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.052 _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 0.25742(5) 0.41642(3) 0.43919(2) 0.03809(19) Uani 1 1 d . . . Mn2 Mn 0.28356(5) 0.36051(3) 0.70815(2) 0.03900(19) Uani 1 1 d . . . C1 C 0.2087(3) 0.2403(2) 0.43636(13) 0.0324(8) Uani 1 1 d . . . C2 C 0.2662(3) 0.1890(2) 0.67231(13) 0.0317(7) Uani 1 1 d . . . C11 C 0.0849(4) 0.2439(3) 0.34517(16) 0.0488(10) Uani 1 1 d . . . H11 H 0.0632 0.1921 0.3406 0.059 Uiso 1 1 calc R . . C12 C 0.0550(5) 0.3014(3) 0.31058(17) 0.0623(13) Uani 1 1 d . . . H12 H 0.0085 0.2977 0.2768 0.075 Uiso 1 1 calc R . . C13 C 0.1057(5) 0.3673(3) 0.33415(17) 0.0577(12) Uani 1 1 d . . . H13 H 0.0987 0.4163 0.3186 0.069 Uiso 1 1 calc R . . C21 C 0.1060(3) 0.2448(2) 0.51691(14) 0.0349(8) Uani 1 1 d . . . H21 H 0.0856 0.1930 0.5197 0.042 Uiso 1 1 calc R . . C22 C 0.0823(3) 0.3027(2) 0.54819(15) 0.0410(9) Uani 1 1 d . . . H22 H 0.0428 0.2994 0.5774 0.049 Uiso 1 1 calc R . . C23 C 0.1266(3) 0.3669(2) 0.52934(14) 0.0374(8) Uani 1 1 d . . . H23 H 0.1218 0.4161 0.5440 0.045 Uiso 1 1 calc R . . C31 C 0.4188(3) 0.2054(2) 0.44012(15) 0.0392(9) Uani 1 1 d . . . H31 H 0.4138 0.1516 0.4376 0.047 Uiso 1 1 calc R . . C32 C 0.5156(4) 0.2486(2) 0.44289(16) 0.0444(9) Uani 1 1 d . . . H32 H 0.5914 0.2308 0.4429 0.053 Uiso 1 1 calc R . . C33 C 0.4810(3) 0.3235(2) 0.44561(15) 0.0399(9) Uani 1 1 d . . . H33 H 0.5312 0.3659 0.4480 0.048 Uiso 1 1 calc R . . C41 C 0.3710(3) 0.2116(2) 0.59469(14) 0.0382(8) Uani 1 1 d . . . H41 H 0.3722 0.1615 0.5812 0.046 Uiso 1 1 calc R . . C42 C 0.4184(4) 0.2745(3) 0.57609(15) 0.0460(10) Uani 1 1 d . . . H42 H 0.4587 0.2772 0.5471 0.055 Uiso 1 1 calc R . . C43 C 0.3953(3) 0.3342(2) 0.60841(14) 0.0422(9) Uani 1 1 d . . . H43 H 0.4182 0.3853 0.6047 0.051 Uiso 1 1 calc R . . C51 C 0.0481(3) 0.1866(2) 0.66339(14) 0.0360(8) Uani 1 1 d . . . H51 H 0.0330 0.1354 0.6529 0.043 Uiso 1 1 calc R . . C52 C -0.0310(3) 0.2396(2) 0.67116(15) 0.0423(9) Uani 1 1 d . . . H52 H -0.1116 0.2332 0.6672 0.051 Uiso 1 1 calc R . . C53 C 0.0318(3) 0.3054(2) 0.68620(15) 0.0397(9) Uani 1 1 d . . . H53 H -0.0010 0.3523 0.6941 0.048 Uiso 1 1 calc R . . C61 C 0.3822(4) 0.1403(3) 0.75868(16) 0.0475(10) Uani 1 1 d . . . H61 H 0.3803 0.0871 0.7523 0.057 Uiso 1 1 calc R . . C62 C 0.4348(4) 0.1769(3) 0.80338(17) 0.0551(12) Uani 1 1 d . . . H62 H 0.4770 0.1543 0.8341 0.066 Uiso 1 1 calc R . . C63 C 0.4140(4) 0.2540(3) 0.79454(15) 0.0492(10) Uani 1 1 d . . . H63 H 0.4410 0.2931 0.8190 0.059 Uiso 1 1 calc R . . C71 C 0.1843(3) 0.1549(2) 0.43503(14) 0.0363(8) Uani 1 1 d . . . H71A H 0.1010 0.1458 0.4317 0.044 Uiso 1 1 calc R . . H71B H 0.2117 0.1315 0.4044 0.044 Uiso 1 1 calc R . . C72 C 0.2300(3) 0.0412(2) 0.48361(16) 0.0378(8) Uani 1 1 d . . . H72A H 0.2888 0.0200 0.5117 0.045 Uiso 1 1 calc R . . H72B H 0.2429 0.0197 0.4495 0.045 Uiso 1 1 calc R . . C73 C 0.1118(3) 0.01817(18) 0.49372(14) 0.0317(7) Uani 1 1 d . . . C74 C 0.0854(3) 0.01185(18) 0.54413(14) 0.0313(7) Uani 1 1 d . . . C75 C 0.0268(3) 0.00655(19) 0.45020(14) 0.0340(8) Uani 1 1 d . . . H75 H 0.0454 0.0112 0.4158 0.041 Uiso 1 1 calc R . . C76 C 0.1733(3) 0.0199(2) 0.59302(15) 0.0363(8) Uani 1 1 d . . . H76A H 0.1466 -0.0062 0.6229 0.044 Uiso 1 1 calc R . . H76B H 0.2460 -0.0040 0.5874 0.044 Uiso 1 1 calc R . . C77 C 0.2599(3) 0.1061(2) 0.65653(14) 0.0364(8) Uani 1 1 d . . . H77A H 0.3379 0.0862 0.6561 0.044 Uiso 1 1 calc R . . H77B H 0.2251 0.0763 0.6825 0.044 Uiso 1 1 calc R . . C81 C 0.3400(4) 0.4671(2) 0.49439(18) 0.0474(10) Uani 1 1 d . . . C82 C 0.3354(4) 0.4660(3) 0.39345(18) 0.0544(11) Uani 1 1 d . . . C83 C 0.1490(4) 0.4898(2) 0.43207(18) 0.0498(10) Uani 1 1 d . . . C91 C 0.2358(4) 0.3957(2) 0.76823(17) 0.0468(10) Uani 1 1 d . . . C92 C 0.4146(4) 0.4166(3) 0.72275(17) 0.0552(12) Uani 1 1 d . . . C93 C 0.2131(4) 0.4383(3) 0.66971(18) 0.0518(11) Uani 1 1 d . . . N11 N 0.1646(3) 0.35138(18) 0.38107(12) 0.0413(8) Uani 1 1 d . . . N12 N 0.1518(3) 0.27505(17) 0.38759(12) 0.0365(7) Uani 1 1 d . . . N21 N 0.1772(3) 0.35179(17) 0.48787(11) 0.0334(7) Uani 1 1 d . . . N22 N 0.1652(2) 0.27581(16) 0.48051(11) 0.0308(6) Uani 1 1 d . . . N31 N 0.3697(3) 0.32827(17) 0.44451(12) 0.0355(7) Uani 1 1 d . . . N32 N 0.3309(3) 0.25496(17) 0.44175(12) 0.0342(7) Uani 1 1 d . . . N41 N 0.3373(3) 0.30998(18) 0.64499(12) 0.0370(7) Uani 1 1 d . . . N42 N 0.3219(3) 0.23437(17) 0.63616(11) 0.0328(7) Uani 1 1 d . . . N51 N 0.1523(3) 0.22039(16) 0.67336(11) 0.0316(6) Uani 1 1 d . . . N52 N 0.1429(3) 0.29395(17) 0.68807(12) 0.0361(7) Uani 1 1 d . . . N61 N 0.3333(3) 0.19568(18) 0.72530(11) 0.0358(7) Uani 1 1 d . . . N62 N 0.3514(3) 0.26560(18) 0.74728(11) 0.0371(7) Uani 1 1 d . . . O1 O 0.2419(2) 0.12283(14) 0.48236(10) 0.0364(6) Uani 1 1 d . . . O2 O 0.1923(2) 0.09860(13) 0.60536(10) 0.0353(6) Uani 1 1 d . . . O81 O 0.3887(3) 0.49807(17) 0.52914(13) 0.0560(8) Uani 1 1 d . . . O82 O 0.3887(4) 0.4951(2) 0.36728(16) 0.0817(12) Uani 1 1 d . . . O83 O 0.0813(3) 0.53569(18) 0.42750(15) 0.0651(9) Uani 1 1 d . . . O91 O 0.2095(3) 0.4146(2) 0.80615(13) 0.0645(9) Uani 1 1 d . . . O92 O 0.4938(3) 0.4519(2) 0.73058(15) 0.0819(12) Uani 1 1 d . . . O93 O 0.1684(4) 0.48535(19) 0.64479(15) 0.0745(11) Uani 1 1 d . . . B1 B 0.0624(9) 0.5282(4) 0.2297(3) 0.096(3) Uani 1 1 d . . . B2 B 0.5028(5) 0.0257(4) 0.3930(3) 0.0645(16) Uani 1 1 d . . . F1 F 0.1770(4) 0.5063(3) 0.24201(16) 0.1335(19) Uani 1 1 d . . . F2 F 0.0099(5) 0.4813(2) 0.1922(2) 0.1362(19) Uani 1 1 d . . . F3 F 0.0567(3) 0.60163(18) 0.21267(15) 0.0931(12) Uani 1 1 d . . . F4 F 0.0097(5) 0.52339(18) 0.27340(16) 0.1262(19) Uani 1 1 d . . . F5 F 0.3926(3) 0.0366(2) 0.39969(18) 0.1017(12) Uani 1 1 d . . . F6 F 0.5369(4) -0.0434(3) 0.4057(3) 0.149(2) Uani 1 1 d . . . F7 F 0.5801(3) 0.0733(2) 0.42577(16) 0.0970(11) Uani 1 1 d . . . F8 F 0.5139(5) 0.0406(6) 0.3446(2) 0.230(4) Uani 1 1 d . . . O1S O 0.2941(11) 0.7842(10) 0.3123(9) 0.56(2) Uani 1 1 d D A 1 C5S C 0.3378(19) 0.7050(14) 0.3136(6) 1.00(6) Uani 1 1 d D A 1 H5S1 H 0.4222 0.7069 0.3169 1.194 Uiso 1 1 calc R A 1 H5S2 H 0.3079 0.6809 0.2793 1.194 Uiso 1 1 calc R A 1 C6S C 0.3075(11) 0.6542(6) 0.3577(12) 0.62(3) Uani 1 1 d D A 1 H6S1 H 0.3070 0.6846 0.3896 0.931 Uiso 1 1 calc R A 1 H6S2 H 0.3644 0.6136 0.3652 0.931 Uiso 1 1 calc R A 1 H6S3 H 0.2315 0.6319 0.3465 0.931 Uiso 1 1 calc R A 1 C7S C 0.3406(9) 0.8466(8) 0.2925(5) 0.214(7) Uani 1 1 d D A 1 H7S1 H 0.3888 0.8280 0.2672 0.257 Uiso 1 1 calc R A 1 H7S2 H 0.3931 0.8700 0.3222 0.257 Uiso 1 1 calc R A 1 C8S C 0.2722(11) 0.9054(6) 0.2672(6) 0.187(6) Uani 1 1 d D A 1 H8S1 H 0.2527 0.8942 0.2294 0.281 Uiso 1 1 calc R A 1 H8S2 H 0.3144 0.9534 0.2721 0.281 Uiso 1 1 calc R A 1 H8S3 H 0.2018 0.9096 0.2824 0.281 Uiso 1 1 calc R A 1 N1S N 0.1183(5) 0.6792(3) 0.0817(3) 0.0999(19) Uani 1 1 d . . . C1S C 0.1872(5) 0.6755(3) 0.1181(3) 0.0696(15) Uani 1 1 d . . . C2S C 0.2748(5) 0.6676(4) 0.1629(3) 0.0829(17) Uani 1 1 d . . . H2S1 H 0.2431 0.6436 0.1917 0.124 Uiso 1 1 calc R . . H2S2 H 0.3052 0.7178 0.1742 0.124 Uiso 1 1 calc R . . H2S3 H 0.3366 0.6360 0.1536 0.124 Uiso 1 1 calc R . . N2S N 0.3122(4) 0.8591(4) 0.1220(2) 0.1000(19) Uani 1 1 d . . . C3S C 0.2293(5) 0.8638(3) 0.0944(2) 0.0641(13) Uani 1 1 d . . . C4S C 0.1248(6) 0.8704(3) 0.0587(3) 0.092(2) Uani 1 1 d . . . H4S1 H 0.0975 0.9229 0.0585 0.138 Uiso 1 1 calc R . . H4S2 H 0.0677 0.8366 0.0699 0.138 Uiso 1 1 calc R . . H4S3 H 0.1370 0.8562 0.0232 0.138 Uiso 1 1 calc R . . N3S N 0.2735(17) 0.8450(6) 0.4434(7) 0.323(12) Uani 1 1 d D B 2 C9S C 0.2652(10) 0.7718(11) 0.4486(5) 0.325(19) Uani 1 1 d D B 2 C10S C 0.2721(14) 0.6815(11) 0.4552(7) 0.280(14) Uani 1 1 d D B 2 H10A H 0.2853 0.6584 0.4220 0.420 Uiso 1 1 calc R B 2 H10B H 0.2000 0.6625 0.4642 0.420 Uiso 1 1 calc R B 2 H10C H 0.3353 0.6683 0.4834 0.420 Uiso 1 1 calc R B 2 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 0.0451(4) 0.0339(3) 0.0365(3) -0.0009(2) 0.0105(3) -0.0054(2) Mn2 0.0484(4) 0.0389(3) 0.0297(3) -0.0042(2) 0.0064(2) -0.0109(3) C1 0.0361(19) 0.0348(19) 0.0263(17) -0.0012(14) 0.0052(14) -0.0032(15) C2 0.0289(18) 0.0390(19) 0.0248(17) 0.0024(14) -0.0025(13) -0.0033(15) C11 0.059(3) 0.051(2) 0.033(2) -0.0081(18) -0.0038(18) -0.003(2) C12 0.094(4) 0.052(3) 0.031(2) -0.0040(19) -0.017(2) 0.000(3) C13 0.085(4) 0.052(3) 0.033(2) 0.0075(19) 0.004(2) 0.005(2) C21 0.0319(19) 0.043(2) 0.0292(18) 0.0078(15) 0.0046(14) -0.0008(16) C22 0.035(2) 0.058(2) 0.032(2) 0.0001(17) 0.0095(16) 0.0021(18) C23 0.040(2) 0.042(2) 0.0311(19) -0.0057(15) 0.0067(15) 0.0006(17) C31 0.038(2) 0.043(2) 0.038(2) -0.0026(16) 0.0106(16) -0.0018(17) C32 0.042(2) 0.049(2) 0.046(2) -0.0007(18) 0.0176(18) -0.0015(18) C33 0.039(2) 0.045(2) 0.039(2) -0.0010(16) 0.0154(17) -0.0097(17) C41 0.032(2) 0.051(2) 0.0310(19) -0.0066(16) 0.0030(15) -0.0007(17) C42 0.043(2) 0.065(3) 0.030(2) -0.0019(18) 0.0068(16) -0.013(2) C43 0.047(2) 0.052(2) 0.0273(19) 0.0004(16) 0.0043(16) -0.0146(19) C51 0.037(2) 0.042(2) 0.0296(18) -0.0018(15) 0.0057(15) -0.0092(17) C52 0.036(2) 0.053(2) 0.037(2) -0.0022(17) 0.0075(16) -0.0045(18) C53 0.041(2) 0.047(2) 0.032(2) -0.0023(16) 0.0105(16) 0.0028(18) C61 0.048(2) 0.052(2) 0.038(2) 0.0110(18) -0.0072(18) -0.004(2) C62 0.054(3) 0.069(3) 0.035(2) 0.010(2) -0.0124(19) -0.008(2) C63 0.047(2) 0.070(3) 0.028(2) -0.0031(18) -0.0021(17) -0.018(2) C71 0.038(2) 0.038(2) 0.0309(19) -0.0012(15) 0.0011(15) -0.0047(16) C72 0.033(2) 0.0338(19) 0.047(2) 0.0030(16) 0.0072(16) -0.0018(15) C73 0.0318(19) 0.0230(16) 0.040(2) -0.0026(14) 0.0037(15) -0.0028(14) C74 0.0334(19) 0.0218(16) 0.0370(19) -0.0026(14) 0.0003(14) -0.0003(14) C75 0.041(2) 0.0290(18) 0.0329(19) -0.0008(14) 0.0093(15) -0.0013(15) C76 0.039(2) 0.0288(18) 0.039(2) -0.0017(15) -0.0010(16) -0.0007(15) C77 0.039(2) 0.0364(19) 0.0310(19) 0.0020(15) -0.0021(15) 0.0003(16) C81 0.051(3) 0.041(2) 0.055(3) 0.001(2) 0.021(2) -0.0041(19) C82 0.071(3) 0.047(2) 0.049(3) 0.002(2) 0.019(2) -0.006(2) C83 0.056(3) 0.042(2) 0.053(3) -0.0045(19) 0.013(2) -0.008(2) C91 0.056(3) 0.044(2) 0.041(2) -0.0064(18) 0.0120(19) -0.0131(19) C92 0.068(3) 0.062(3) 0.038(2) -0.010(2) 0.016(2) -0.021(2) C93 0.072(3) 0.041(2) 0.043(2) -0.0035(19) 0.013(2) -0.014(2) N11 0.053(2) 0.0381(17) 0.0315(17) 0.0021(13) 0.0040(14) -0.0017(15) N12 0.0474(19) 0.0342(16) 0.0273(15) -0.0020(12) 0.0045(13) -0.0053(14) N21 0.0365(17) 0.0347(16) 0.0288(15) -0.0038(12) 0.0055(12) -0.0036(13) N22 0.0325(16) 0.0328(15) 0.0264(15) -0.0018(12) 0.0026(12) -0.0059(12) N31 0.0416(18) 0.0333(16) 0.0332(16) -0.0020(12) 0.0105(13) -0.0076(13) N32 0.0365(17) 0.0323(16) 0.0347(16) -0.0041(12) 0.0087(13) -0.0062(13) N41 0.0413(18) 0.0384(17) 0.0307(16) 0.0005(13) 0.0042(13) -0.0077(14) N42 0.0336(16) 0.0360(16) 0.0280(15) -0.0021(12) 0.0021(12) -0.0050(13) N51 0.0340(16) 0.0336(15) 0.0267(15) -0.0006(12) 0.0037(12) -0.0018(13) N52 0.0440(19) 0.0342(16) 0.0292(16) -0.0030(12) 0.0035(13) -0.0033(14) N61 0.0377(17) 0.0441(17) 0.0226(15) 0.0034(12) -0.0041(12) -0.0079(14) N62 0.0389(18) 0.0453(18) 0.0257(15) -0.0007(13) 0.0006(13) -0.0106(14) O1 0.0379(14) 0.0361(14) 0.0330(13) 0.0024(10) -0.0005(11) -0.0085(11) O2 0.0410(14) 0.0307(13) 0.0310(13) -0.0022(10) -0.0036(10) -0.0031(11) O81 0.069(2) 0.0458(17) 0.0522(19) -0.0143(14) 0.0075(16) -0.0234(16) O82 0.102(3) 0.071(2) 0.083(3) 0.020(2) 0.048(2) -0.009(2) O83 0.061(2) 0.0456(18) 0.089(3) -0.0035(17) 0.0123(18) 0.0062(16) O91 0.075(2) 0.072(2) 0.0495(19) -0.0186(16) 0.0195(17) -0.0154(18) O92 0.082(3) 0.096(3) 0.071(2) -0.027(2) 0.024(2) -0.057(2) O93 0.107(3) 0.0480(19) 0.064(2) 0.0146(17) 0.003(2) -0.005(2) B1 0.163(8) 0.061(4) 0.082(5) 0.016(4) 0.073(5) 0.059(5) B2 0.054(3) 0.073(4) 0.071(4) -0.006(3) 0.022(3) 0.019(3) F1 0.174(4) 0.147(4) 0.084(3) 0.011(2) 0.036(3) 0.114(4) F2 0.189(5) 0.090(3) 0.152(4) -0.035(3) 0.093(4) 0.020(3) F3 0.103(3) 0.070(2) 0.120(3) 0.0424(19) 0.056(2) 0.0281(18) F4 0.233(5) 0.063(2) 0.113(3) 0.028(2) 0.119(3) 0.054(3) F5 0.062(2) 0.104(3) 0.148(3) -0.028(2) 0.040(2) 0.0184(19) F6 0.095(3) 0.096(3) 0.250(6) -0.034(3) 0.006(3) 0.045(3) F7 0.073(2) 0.102(3) 0.112(3) -0.019(2) 0.001(2) 0.028(2) F8 0.134(5) 0.480(13) 0.074(3) 0.044(5) 0.013(3) -0.089(6) O1S 0.178(10) 0.66(4) 0.79(4) 0.57(4) -0.092(17) -0.133(16) C5S 0.79(6) 1.88(13) 0.191(18) -0.42(4) -0.27(3) 1.15(8) C6S 0.088(8) 0.080(7) 1.66(10) -0.21(2) 0.05(3) 0.013(6) C7S 0.120(9) 0.312(19) 0.207(13) 0.096(13) 0.018(9) -0.094(11) C8S 0.173(12) 0.125(9) 0.256(17) 0.033(9) 0.014(11) 0.018(8) N1S 0.082(4) 0.064(3) 0.141(6) 0.005(3) -0.018(4) -0.001(3) C1S 0.057(3) 0.052(3) 0.099(5) -0.003(3) 0.011(3) -0.006(3) C2S 0.068(4) 0.084(4) 0.093(5) 0.002(3) 0.004(3) -0.017(3) N2S 0.056(3) 0.139(5) 0.100(4) -0.018(4) -0.001(3) 0.026(3) C3S 0.053(3) 0.065(3) 0.073(4) -0.009(3) 0.008(3) 0.006(2) C4S 0.092(5) 0.071(4) 0.098(5) 0.000(3) -0.029(4) 0.002(3) N3S 0.51(3) 0.114(7) 0.301(18) -0.101(10) -0.074(17) 0.120(11) C9S 0.089(8) 0.79(6) 0.088(9) -0.11(2) 0.005(6) -0.047(19) C10S 0.215(17) 0.42(3) 0.168(13) 0.086(16) -0.079(11) -0.22(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 C83 1.809(5) . ? Mn1 C81 1.818(5) . ? Mn1 C82 1.832(4) . ? Mn1 N31 2.035(3) . ? Mn1 N21 2.039(3) . ? Mn1 N11 2.051(3) . ? Mn2 C93 1.810(5) . ? Mn2 C92 1.827(5) . ? Mn2 C91 1.837(4) . ? Mn2 N52 2.033(3) . ? Mn2 N41 2.043(3) . ? Mn2 N62 2.046(3) . ? C1 N32 1.455(5) . ? C1 N12 1.455(5) . ? C1 N22 1.461(4) . ? C1 C71 1.532(5) . ? C2 N51 1.462(5) . ? C2 N61 1.463(4) . ? C2 N42 1.464(4) . ? C2 C77 1.515(5) . ? C11 N12 1.353(5) . ? C11 C12 1.357(6) . ? C12 C13 1.397(7) . ? C13 N11 1.319(5) . ? C21 C22 1.357(5) . ? C21 N22 1.372(4) . ? C22 C23 1.369(6) . ? C23 N21 1.333(4) . ? C31 N32 1.365(5) . ? C31 C32 1.369(6) . ? C32 C33 1.388(6) . ? C33 N31 1.317(5) . ? C41 N42 1.356(5) . ? C41 C42 1.364(6) . ? C42 C43 1.394(6) . ? C43 N41 1.323(5) . ? C51 N51 1.356(5) . ? C51 C52 1.360(6) . ? C52 C53 1.396(6) . ? C53 N52 1.324(5) . ? C61 N61 1.364(5) . ? C61 C62 1.374(6) . ? C62 C63 1.393(7) . ? C63 N62 1.329(5) . ? C71 O1 1.410(4) . ? C72 O1 1.447(4) . ? C72 C73 1.520(5) . ? C73 C74 1.386(5) . ? C73 C75 1.390(5) . ? C74 C75 1.399(5) 3_556 ? C74 C76 1.500(5) . ? C75 C74 1.399(5) 3_556 ? C76 O2 1.432(4) . ? C77 O2 1.427(4) . ? C81 O81 1.121(5) . ? C82 O82 1.119(5) . ? C83 O83 1.132(5) . ? C91 O91 1.121(5) . ? C92 O92 1.115(5) . ? C93 O93 1.125(6) . ? N11 N12 1.367(4) . ? N21 N22 1.357(4) . ? N31 N32 1.369(4) . ? N41 N42 1.359(4) . ? N51 N52 1.360(4) . ? N61 N62 1.358(4) . ? B1 F2 1.341(11) . ? B1 F3 1.364(7) . ? B1 F4 1.373(7) . ? B1 F1 1.396(10) . ? B2 F8 1.299(8) . ? B2 F6 1.309(8) . ? B2 F5 1.357(7) . ? B2 F7 1.413(8) . ? O1S C7S 1.366(8) . ? O1S C5S 1.486(10) . ? C5S C6S 1.533(10) . ? C7S C8S 1.408(8) . ? N1S C1S 1.136(8) . ? C1S C2S 1.423(9) . ? N2S C3S 1.114(7) . ? C3S C4S 1.417(8) . ? N3S C9S 1.301(17) . ? C9S C10S 1.602(16) . ? 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 C83 Mn1 C81 90.5(2) . . ? C83 Mn1 C82 91.1(2) . . ? C81 Mn1 C82 90.1(2) . . ? C83 Mn1 N31 175.54(17) . . ? C81 Mn1 N31 93.53(16) . . ? C82 Mn1 N31 90.78(17) . . ? C83 Mn1 N21 93.80(16) . . ? C81 Mn1 N21 92.37(15) . . ? C82 Mn1 N21 174.46(17) . . ? N31 Mn1 N21 84.15(12) . . ? C83 Mn1 N11 92.28(17) . . ? C81 Mn1 N11 175.12(16) . . ? C82 Mn1 N11 93.80(18) . . ? N31 Mn1 N11 83.56(13) . . ? N21 Mn1 N11 83.46(12) . . ? C93 Mn2 C92 90.1(2) . . ? C93 Mn2 C91 91.4(2) . . ? C92 Mn2 C91 90.82(19) . . ? C93 Mn2 N52 90.81(17) . . ? C92 Mn2 N52 175.95(16) . . ? C91 Mn2 N52 93.11(16) . . ? C93 Mn2 N41 94.19(16) . . ? C92 Mn2 N41 91.90(16) . . ? C91 Mn2 N41 173.78(16) . . ? N52 Mn2 N41 84.09(12) . . ? C93 Mn2 N62 174.26(17) . . ? C92 Mn2 N62 95.20(19) . . ? C91 Mn2 N62 90.79(17) . . ? N52 Mn2 N62 83.78(12) . . ? N41 Mn2 N62 83.40(12) . . ? N32 C1 N12 108.6(3) . . ? N32 C1 N22 108.8(3) . . ? N12 C1 N22 108.4(3) . . ? N32 C1 C71 110.9(3) . . ? N12 C1 C71 109.6(3) . . ? N22 C1 C71 110.4(3) . . ? N51 C2 N61 108.3(3) . . ? N51 C2 N42 108.6(3) . . ? N61 C2 N42 108.2(3) . . ? N51 C2 C77 111.4(3) . . ? N61 C2 C77 108.8(3) . . ? N42 C2 C77 111.4(3) . . ? N12 C11 C12 106.1(4) . . ? C11 C12 C13 106.9(4) . . ? N11 C13 C12 110.1(4) . . ? C22 C21 N22 106.5(3) . . ? C21 C22 C23 106.5(3) . . ? N21 C23 C22 111.5(3) . . ? N32 C31 C32 106.2(3) . . ? C31 C32 C33 106.3(4) . . ? N31 C33 C32 111.3(3) . . ? N42 C41 C42 106.8(3) . . ? C41 C42 C43 105.8(3) . . ? N41 C43 C42 110.9(4) . . ? N51 C51 C52 107.4(3) . . ? C51 C52 C53 105.2(3) . . ? N52 C53 C52 111.3(3) . . ? N61 C61 C62 106.0(4) . . ? C61 C62 C63 106.2(4) . . ? N62 C63 C62 110.8(4) . . ? O1 C71 C1 108.2(3) . . ? O1 C72 C73 111.4(3) . . ? C74 C73 C75 119.6(3) . . ? C74 C73 C72 122.5(3) . . ? C75 C73 C72 117.8(3) . . ? C73 C74 C75 118.8(3) . 3_556 ? C73 C74 C76 122.8(3) . . ? C75 C74 C76 118.4(3) 3_556 . ? C73 C75 C74 121.7(3) . 3_556 ? O2 C76 C74 109.8(3) . . ? O2 C77 C2 109.3(3) . . ? O81 C81 Mn1 178.2(4) . . ? O82 C82 Mn1 176.1(5) . . ? O83 C83 Mn1 179.8(5) . . ? O91 C91 Mn2 176.8(4) . . ? O92 C92 Mn2 178.3(5) . . ? O93 C93 Mn2 178.2(4) . . ? C13 N11 N12 105.6(3) . . ? C13 N11 Mn1 133.2(3) . . ? N12 N11 Mn1 121.2(2) . . ? C11 N12 N11 111.3(3) . . ? C11 N12 C1 130.4(3) . . ? N11 N12 C1 118.3(3) . . ? C23 N21 N22 105.0(3) . . ? C23 N21 Mn1 134.0(3) . . ? N22 N21 Mn1 121.0(2) . . ? N21 N22 C21 110.6(3) . . ? N21 N22 C1 119.2(3) . . ? C21 N22 C1 130.1(3) . . ? C33 N31 N32 105.5(3) . . ? C33 N31 Mn1 133.7(3) . . ? N32 N31 Mn1 120.5(2) . . ? C31 N32 N31 110.8(3) . . ? C31 N32 C1 129.5(3) . . ? N31 N32 C1 119.5(3) . . ? C43 N41 N42 105.6(3) . . ? C43 N41 Mn2 133.7(3) . . ? N42 N41 Mn2 120.6(2) . . ? C41 N42 N41 111.0(3) . . ? C41 N42 C2 129.4(3) . . ? N41 N42 C2 119.5(3) . . ? C51 N51 N52 110.8(3) . . ? C51 N51 C2 130.1(3) . . ? N52 N51 C2 119.0(3) . . ? C53 N52 N51 105.2(3) . . ? C53 N52 Mn2 133.6(3) . . ? N51 N52 Mn2 121.2(2) . . ? N62 N61 C61 111.5(3) . . ? N62 N61 C2 119.0(3) . . ? C61 N61 C2 129.5(3) . . ? C63 N62 N61 105.5(3) . . ? C63 N62 Mn2 133.5(3) . . ? N61 N62 Mn2 121.0(2) . . ? C71 O1 C72 112.5(3) . . ? C77 O2 C76 109.7(3) . . ? F2 B1 F3 111.1(7) . . ? F2 B1 F4 109.3(8) . . ? F3 B1 F4 108.4(4) . . ? F2 B1 F1 108.0(5) . . ? F3 B1 F1 109.2(7) . . ? F4 B1 F1 110.8(6) . . ? F8 B2 F6 110.5(7) . . ? F8 B2 F5 110.2(6) . . ? F6 B2 F5 111.3(6) . . ? F8 B2 F7 107.0(6) . . ? F6 B2 F7 105.1(5) . . ? F5 B2 F7 112.6(5) . . ? C7S O1S C5S 127(2) . . ? O1S C5S C6S 116.2(13) . . ? O1S C7S C8S 121.9(11) . . ? N1S C1S C2S 177.4(7) . . ? N2S C3S C4S 179.2(8) . . ? N3S C9S C10S 172.8(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn1 N11 N12 C11 178.2(3) . . . . ? Mn1 N21 N22 C21 -178.3(2) . . . . ? Mn1 N31 N32 C31 173.1(2) . . . . ? Mn2 N41 N42 C41 -175.5(2) . . . . ? Mn2 N51 N52 C51 -178.1(2) . . . . ? Mn2 N61 N62 C61 177.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.908 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.095