# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1771 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Michael W. Day Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; _publ_contact_author_phone '(818) 395 2734' _publ_contact_author_fax '(818) 449 4159' _publ_contact_author_email mike@xray.caltech.edu _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _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 ; ; # 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 'Day, Michael W.' #<--'Last name, first name' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Bendix, Jesper' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Gross, Zev' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Gray, Harry B.' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== # 5. CHEMICAL DATA data_zig1t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H23 F15 Mn N4 O P' _chemical_formula_weight 1126.68 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8826(15) _cell_length_b 12.8019(14) _cell_length_c 25.952(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.306(2) _cell_angle_gamma 90.00 _cell_volume 4537.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 4520 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.53 _exptl_crystal_description Plate _exptl_crystal_colour Purple _exptl_crystal_size_max 0.222 _exptl_crystal_size_mid 0.185 _exptl_crystal_size_min 0.007 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29363 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1420 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.60 _reflns_number_total 10384 _reflns_number_gt 5262 _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Direct methods' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10384 _refine_ls_number_parameters 786 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1167 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.857 _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 Mn Mn 0.75325(3) 0.87126(3) 0.157843(18) 0.01615(11) Uani 1 1 d . . . P P 0.75694(6) 1.08256(6) 0.07170(3) 0.0196(2) Uani 1 1 d . . . O O 0.75560(15) 0.97831(14) 0.09806(7) 0.0208(5) Uani 1 1 d . . . F1 F 0.95853(13) 0.71097(14) 0.01826(6) 0.0298(5) Uani 1 1 d . . . F2 F 1.09525(13) 0.59290(14) -0.01450(7) 0.0340(5) Uani 1 1 d . . . F3 F 1.20573(13) 0.45831(13) 0.05240(7) 0.0348(5) Uani 1 1 d . . . F4 F 1.17943(13) 0.44539(14) 0.15329(7) 0.0349(5) Uani 1 1 d . . . F5 F 1.04191(12) 0.56027(13) 0.18645(6) 0.0271(4) Uani 1 1 d . . . F6 F 0.92363(13) 0.94867(13) 0.36141(6) 0.0265(4) Uani 1 1 d . . . F7 F 1.06512(13) 1.03219(13) 0.43453(7) 0.0318(5) Uani 1 1 d . . . F8 F 1.20263(13) 1.15806(13) 0.40524(7) 0.0342(5) Uani 1 1 d . . . F9 F 1.19683(13) 1.20358(14) 0.30289(7) 0.0344(5) Uani 1 1 d . . . F10 F 1.05095(12) 1.12594(13) 0.22966(6) 0.0260(4) Uani 1 1 d . . . F11 F 0.54489(12) 1.20938(12) 0.16439(6) 0.0242(4) Uani 1 1 d . . . F12 F 0.37892(13) 1.32058(12) 0.15673(7) 0.0289(5) Uani 1 1 d . . . F13 F 0.21682(13) 1.23348(14) 0.18399(8) 0.0386(5) Uani 1 1 d . . . F14 F 0.22207(13) 1.03126(13) 0.21760(7) 0.0337(5) Uani 1 1 d . . . F15 F 0.38418(12) 0.91722(12) 0.22181(6) 0.0235(4) Uani 1 1 d . . . N1 N 0.89042(17) 0.84749(17) 0.18291(9) 0.0150(6) Uani 1 1 d . . . N2 N 0.73558(17) 0.96690(18) 0.21234(9) 0.0164(6) Uani 1 1 d . . . N3 N 0.61511(17) 0.84661(17) 0.14364(9) 0.0160(6) Uani 1 1 d . . . N4 N 0.74965(18) 0.74870(18) 0.11554(9) 0.0181(6) Uani 1 1 d . . . C1 C 0.9519(2) 0.7807(2) 0.16157(11) 0.0169(7) Uani 1 1 d . . . C2 C 1.0492(2) 0.8009(2) 0.18767(12) 0.0190(7) Uani 1 1 d . . . C3 C 1.0469(2) 0.8760(2) 0.22409(12) 0.0179(7) Uani 1 1 d . . . C4 C 0.9474(2) 0.9062(2) 0.22138(11) 0.0164(7) Uani 1 1 d . . . C5 C 0.9096(2) 0.9813(2) 0.25206(11) 0.0171(7) Uani 1 1 d . . . C6 C 0.8110(2) 1.0097(2) 0.24844(11) 0.0164(7) Uani 1 1 d . . . C7 C 0.7698(2) 1.0870(2) 0.27819(12) 0.0186(7) Uani 1 1 d . . . C8 C 0.6716(2) 1.0908(2) 0.25971(12) 0.0201(7) Uani 1 1 d . . . C9 C 0.6487(2) 1.0157(2) 0.21850(11) 0.0178(7) Uani 1 1 d . . . C10 C 0.5567(2) 0.9919(2) 0.18851(11) 0.0168(7) Uani 1 1 d . . . C11 C 0.5398(2) 0.9093(2) 0.15173(11) 0.0179(7) Uani 1 1 d . . . C12 C 0.4542(2) 0.8755(2) 0.11699(12) 0.0183(7) Uani 1 1 d . . . C13 C 0.4808(2) 0.7944(2) 0.08732(12) 0.0185(7) Uani 1 1 d . . . C14 C 0.5822(2) 0.7766(2) 0.10431(11) 0.0172(7) Uani 1 1 d . . . C15 C 0.6588(2) 0.7159(2) 0.09039(11) 0.0180(7) Uani 1 1 d . . . C16 C 0.6738(2) 0.6276(2) 0.05964(12) 0.0213(7) Uani 1 1 d . . . C17 C 0.7716(2) 0.6091(2) 0.06651(12) 0.0222(8) Uani 1 1 d . . . C18 C 0.8204(2) 0.6878(2) 0.10125(11) 0.0164(7) Uani 1 1 d . . . C19 C 0.9197(2) 0.7058(2) 0.12297(11) 0.0182(7) Uani 1 1 d . . . C20 C 0.9950(2) 0.6398(2) 0.10358(11) 0.0180(7) Uani 1 1 d . . . C21 C 1.0106(2) 0.6450(2) 0.05283(12) 0.0210(7) Uani 1 1 d . . . C22 C 1.0808(2) 0.5844(2) 0.03474(12) 0.0224(8) Uani 1 1 d . . . C23 C 1.1367(2) 0.5163(2) 0.06881(13) 0.0237(8) Uani 1 1 d . . . C24 C 1.1239(2) 0.5105(2) 0.11954(13) 0.0243(8) Uani 1 1 d . . . C25 C 1.0532(2) 0.5708(2) 0.13622(12) 0.0220(8) Uani 1 1 d . . . C26 C 0.9828(2) 1.0333(2) 0.29310(12) 0.0175(7) Uani 1 1 d . . . C27 C 0.9890(2) 1.0128(2) 0.34580(12) 0.0209(7) Uani 1 1 d . . . C28 C 1.0616(2) 1.0530(2) 0.38341(12) 0.0233(8) Uani 1 1 d . . . C29 C 1.1319(2) 1.1172(2) 0.36833(13) 0.0242(8) Uani 1 1 d . . . C30 C 1.1281(2) 1.1409(2) 0.31656(13) 0.0225(8) Uani 1 1 d . . . C31 C 1.0541(2) 1.1006(2) 0.27991(12) 0.0194(7) Uani 1 1 d . . . C32 C 0.4706(2) 1.0579(2) 0.19256(11) 0.0164(7) Uani 1 1 d . . . C33 C 0.4654(2) 1.1633(2) 0.17695(12) 0.0195(7) Uani 1 1 d . . . C34 C 0.3817(2) 1.2210(2) 0.17375(12) 0.0207(7) Uani 1 1 d . . . C35 C 0.2993(2) 1.1775(2) 0.18724(13) 0.0243(8) Uani 1 1 d . . . C36 C 0.3021(2) 1.0751(2) 0.20362(12) 0.0230(8) Uani 1 1 d . . . C37 C 0.3859(2) 1.0182(2) 0.20561(12) 0.0193(7) Uani 1 1 d . . . C38 C 0.8326(2) 1.1769(2) 0.11003(12) 0.0219(8) Uani 1 1 d . . . C39 C 0.9228(3) 1.2066(3) 0.09832(15) 0.0330(9) Uani 1 1 d . . . C40 C 0.9803(3) 1.2790(3) 0.13052(16) 0.0409(11) Uani 1 1 d . . . C41 C 0.9498(3) 1.3181(3) 0.17434(16) 0.0450(11) Uani 1 1 d . . . C42 C 0.8610(3) 1.2875(3) 0.18655(15) 0.0372(10) Uani 1 1 d . . . C43 C 0.8036(3) 1.2167(3) 0.15447(14) 0.0310(9) Uani 1 1 d . . . C44 C 0.6372(2) 1.1393(2) 0.05814(11) 0.0192(7) Uani 1 1 d . . . C45 C 0.5562(3) 1.0736(3) 0.05365(12) 0.0251(8) Uani 1 1 d . . . C46 C 0.4620(3) 1.1144(3) 0.04476(12) 0.0295(9) Uani 1 1 d . . . C47 C 0.4486(3) 1.2218(3) 0.04010(13) 0.0329(9) Uani 1 1 d . . . C48 C 0.5280(3) 1.2872(3) 0.04467(13) 0.0312(9) Uani 1 1 d . . . C49 C 0.6224(3) 1.2477(2) 0.05356(12) 0.0253(8) Uani 1 1 d . . . C50 C 0.7996(2) 1.0630(2) 0.01077(12) 0.0218(7) Uani 1 1 d . . . C51 C 0.7976(2) 1.1425(3) -0.02637(13) 0.0261(8) Uani 1 1 d . . . C52 C 0.8299(3) 1.1227(3) -0.07248(13) 0.0328(9) Uani 1 1 d . . . C53 C 0.8630(3) 1.0259(3) -0.08312(15) 0.0388(10) Uani 1 1 d . . . C54 C 0.8642(3) 0.9466(3) -0.04699(15) 0.0468(11) Uani 1 1 d . . . C55 C 0.8320(3) 0.9644(3) 0.00016(14) 0.0351(9) Uani 1 1 d . . . H2 H 1.1021(18) 0.7699(18) 0.1803(9) 0.001(7) Uiso 1 1 d . . . H3 H 1.0905(19) 0.905(2) 0.2472(10) 0.017(9) Uiso 1 1 d . . . H7 H 0.806(2) 1.125(2) 0.3088(10) 0.023(8) Uiso 1 1 d . . . H8 H 0.622(2) 1.126(2) 0.2699(10) 0.017(8) Uiso 1 1 d . . . H12 H 0.3891(18) 0.9075(18) 0.1131(9) 0.003(7) Uiso 1 1 d . . . H13 H 0.442(2) 0.760(2) 0.0587(10) 0.019(8) Uiso 1 1 d . . . H16 H 0.6268(19) 0.5902(19) 0.0377(10) 0.014(8) Uiso 1 1 d . . . H17 H 0.807(2) 0.555(2) 0.0525(11) 0.024(9) Uiso 1 1 d . . . H39 H 0.941(2) 1.182(3) 0.0672(13) 0.047(12) Uiso 1 1 d . . . H40 H 1.045(3) 1.298(3) 0.1241(13) 0.061(13) Uiso 1 1 d . . . H41 H 0.995(2) 1.363(2) 0.1981(12) 0.045(11) Uiso 1 1 d . . . H42 H 0.830(3) 1.318(3) 0.2143(13) 0.056(12) Uiso 1 1 d . . . H43 H 0.744(3) 1.196(3) 0.1633(13) 0.058(13) Uiso 1 1 d . . . H45 H 0.570(2) 1.000(2) 0.0569(10) 0.019(8) Uiso 1 1 d . . . H46 H 0.398(2) 1.068(2) 0.0384(11) 0.039(10) Uiso 1 1 d . . . H47 H 0.379(2) 1.254(2) 0.0309(11) 0.032(9) Uiso 1 1 d . . . H48 H 0.520(2) 1.362(2) 0.0413(11) 0.033(10) Uiso 1 1 d . . . H49 H 0.6815(19) 1.2929(19) 0.0587(9) 0.010(8) Uiso 1 1 d . . . H51 H 0.7737(19) 1.208(2) -0.0187(10) 0.013(8) Uiso 1 1 d . . . H52 H 0.825(2) 1.179(2) -0.0956(12) 0.035(10) Uiso 1 1 d . . . H53 H 0.887(2) 1.015(2) -0.1125(12) 0.038(11) Uiso 1 1 d . . . H54 H 0.875(2) 0.874(2) -0.0589(12) 0.044(10) Uiso 1 1 d . . . H55 H 0.837(2) 0.913(2) 0.0275(12) 0.047(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0139(3) 0.0165(2) 0.0185(2) -0.0017(2) 0.0038(2) 0.0003(2) P 0.0209(5) 0.0184(4) 0.0197(4) 0.0006(4) 0.0041(4) -0.0010(4) O 0.0228(13) 0.0166(11) 0.0234(12) 0.0052(9) 0.0054(10) 0.0010(10) F1 0.0335(12) 0.0353(11) 0.0217(10) 0.0061(9) 0.0075(9) 0.0097(10) F2 0.0395(13) 0.0385(11) 0.0282(11) -0.0048(9) 0.0178(10) 0.0023(10) F3 0.0299(12) 0.0341(11) 0.0442(13) -0.0082(10) 0.0168(10) 0.0093(10) F4 0.0318(12) 0.0307(11) 0.0419(12) 0.0050(9) 0.0056(10) 0.0146(10) F5 0.0307(12) 0.0272(10) 0.0243(10) 0.0040(8) 0.0074(9) 0.0070(9) F6 0.0272(11) 0.0300(11) 0.0229(10) 0.0004(8) 0.0058(9) -0.0062(9) F7 0.0334(12) 0.0357(11) 0.0238(11) -0.0014(9) -0.0013(9) -0.0004(10) F8 0.0197(11) 0.0328(11) 0.0454(12) -0.0158(9) -0.0068(10) 0.0016(9) F9 0.0197(11) 0.0280(11) 0.0565(14) -0.0034(10) 0.0093(10) -0.0075(9) F10 0.0223(11) 0.0288(10) 0.0289(11) 0.0027(9) 0.0096(9) -0.0002(9) F11 0.0210(11) 0.0219(9) 0.0322(11) 0.0009(8) 0.0119(9) -0.0029(9) F12 0.0328(12) 0.0184(9) 0.0365(12) 0.0062(8) 0.0084(10) 0.0069(9) F13 0.0229(12) 0.0333(11) 0.0623(14) 0.0104(10) 0.0145(11) 0.0138(10) F14 0.0197(11) 0.0332(11) 0.0524(13) 0.0053(10) 0.0181(10) 0.0013(9) F15 0.0186(10) 0.0201(9) 0.0341(11) 0.0069(8) 0.0112(9) 0.0016(8) N1 0.0153(15) 0.0149(13) 0.0159(13) -0.0022(10) 0.0055(11) 0.0019(11) N2 0.0102(14) 0.0187(14) 0.0204(14) -0.0010(11) 0.0030(11) 0.0013(11) N3 0.0143(15) 0.0163(13) 0.0177(14) -0.0034(10) 0.0034(12) -0.0007(11) N4 0.0143(15) 0.0174(13) 0.0219(15) -0.0018(11) 0.0013(12) 0.0015(12) C1 0.0189(19) 0.0171(16) 0.0156(16) 0.0024(13) 0.0059(14) 0.0035(14) C2 0.018(2) 0.0219(18) 0.0190(17) 0.0014(14) 0.0080(15) 0.0031(16) C3 0.0148(18) 0.0168(16) 0.0219(18) 0.0011(15) 0.0029(15) -0.0011(15) C4 0.0100(17) 0.0184(16) 0.0215(17) -0.0014(13) 0.0042(14) -0.0014(13) C5 0.0165(18) 0.0180(17) 0.0162(16) -0.0019(13) 0.0009(14) -0.0018(14) C6 0.0145(18) 0.0187(16) 0.0161(16) 0.0004(13) 0.0031(14) 0.0004(14) C7 0.0181(19) 0.0204(17) 0.0175(17) -0.0021(14) 0.0033(14) 0.0033(15) C8 0.019(2) 0.0242(18) 0.0191(18) -0.0025(14) 0.0086(15) 0.0046(16) C9 0.0150(18) 0.0178(17) 0.0206(17) -0.0016(13) 0.0029(14) 0.0015(14) C10 0.0158(18) 0.0190(16) 0.0168(16) 0.0023(13) 0.0062(14) 0.0021(14) C11 0.0169(18) 0.0171(16) 0.0213(17) 0.0019(13) 0.0081(14) 0.0009(14) C12 0.0161(18) 0.0174(16) 0.0209(17) 0.0029(14) 0.0019(14) 0.0014(15) C13 0.0146(18) 0.0186(17) 0.0224(18) -0.0003(14) 0.0039(15) -0.0004(15) C14 0.0174(19) 0.0187(16) 0.0156(16) 0.0008(13) 0.0028(14) 0.0004(14) C15 0.0185(19) 0.0189(16) 0.0166(16) 0.0019(13) 0.0027(14) 0.0012(15) C16 0.022(2) 0.0198(17) 0.0211(18) -0.0036(15) 0.0003(15) -0.0017(16) C17 0.027(2) 0.0172(18) 0.0223(18) -0.0034(14) 0.0045(16) 0.0010(16) C18 0.0188(19) 0.0154(16) 0.0157(16) 0.0001(13) 0.0049(14) 0.0006(14) C19 0.0193(19) 0.0191(17) 0.0176(17) 0.0034(13) 0.0070(14) 0.0059(15) C20 0.0136(17) 0.0183(16) 0.0224(17) -0.0012(14) 0.0042(14) -0.0033(14) C21 0.0212(19) 0.0187(17) 0.0227(18) -0.0009(14) 0.0029(15) 0.0008(15) C22 0.025(2) 0.0252(18) 0.0188(18) -0.0055(15) 0.0088(15) -0.0030(16) C23 0.0144(19) 0.0228(18) 0.035(2) -0.0082(15) 0.0074(16) 0.0020(15) C24 0.020(2) 0.0233(18) 0.0277(19) 0.0014(15) -0.0002(16) 0.0041(15) C25 0.025(2) 0.0220(17) 0.0193(18) -0.0030(14) 0.0049(15) -0.0017(15) C26 0.0095(17) 0.0173(16) 0.0247(18) -0.0041(13) 0.0001(14) 0.0017(14) C27 0.0153(19) 0.0208(17) 0.0281(19) -0.0021(14) 0.0079(15) -0.0026(15) C28 0.025(2) 0.0223(18) 0.0211(18) -0.0032(14) 0.0004(16) 0.0046(16) C29 0.0134(18) 0.0231(18) 0.033(2) -0.0101(15) -0.0046(16) 0.0037(15) C30 0.0127(18) 0.0165(17) 0.039(2) -0.0018(15) 0.0062(16) 0.0017(14) C31 0.0177(19) 0.0180(17) 0.0234(18) 0.0011(13) 0.0056(15) 0.0055(14) C32 0.0144(18) 0.0180(16) 0.0176(16) -0.0031(13) 0.0048(14) 0.0003(14) C33 0.0149(19) 0.0225(17) 0.0223(18) 0.0007(14) 0.0066(15) -0.0024(14) C34 0.021(2) 0.0162(17) 0.0252(18) 0.0024(14) 0.0042(15) 0.0017(15) C35 0.0122(19) 0.0267(19) 0.034(2) 0.0013(15) 0.0038(16) 0.0095(15) C36 0.0150(19) 0.0258(19) 0.0305(19) 0.0022(15) 0.0101(15) -0.0033(16) C37 0.0158(18) 0.0182(17) 0.0237(18) 0.0015(14) 0.0026(15) -0.0004(14) C38 0.021(2) 0.0221(17) 0.0217(18) 0.0030(14) 0.0006(15) -0.0001(15) C39 0.027(2) 0.033(2) 0.037(2) -0.0003(18) -0.0012(19) -0.0009(18) C40 0.030(3) 0.041(2) 0.046(3) 0.013(2) -0.009(2) -0.014(2) C41 0.061(3) 0.030(2) 0.035(2) 0.0025(19) -0.015(2) -0.013(2) C42 0.046(3) 0.028(2) 0.033(2) -0.0082(18) -0.003(2) -0.005(2) C43 0.030(2) 0.032(2) 0.030(2) -0.0020(16) 0.0005(18) -0.0012(19) C44 0.0225(19) 0.0231(17) 0.0114(15) 0.0005(13) 0.0016(14) 0.0010(16) C45 0.025(2) 0.0253(19) 0.0248(19) -0.0009(16) 0.0048(16) -0.0004(17) C46 0.019(2) 0.045(2) 0.0239(19) -0.0001(17) 0.0034(16) 0.0027(19) C47 0.032(2) 0.043(2) 0.023(2) 0.0051(17) 0.0030(17) 0.013(2) C48 0.035(2) 0.035(2) 0.024(2) -0.0015(17) 0.0061(17) 0.013(2) C49 0.027(2) 0.028(2) 0.0198(18) -0.0020(15) 0.0008(16) 0.0007(17) C50 0.0177(19) 0.0232(18) 0.0240(18) 0.0006(14) 0.0028(15) -0.0003(15) C51 0.024(2) 0.029(2) 0.0262(19) 0.0034(16) 0.0072(16) 0.0011(17) C52 0.032(2) 0.045(2) 0.024(2) 0.0113(18) 0.0110(17) 0.000(2) C53 0.038(3) 0.055(3) 0.028(2) 0.001(2) 0.018(2) 0.004(2) C54 0.065(3) 0.039(2) 0.042(3) 0.000(2) 0.028(2) 0.015(2) C55 0.045(3) 0.033(2) 0.032(2) 0.0067(17) 0.0197(19) 0.0121(19) _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 Mn N4 1.910(2) . yes Mn N2 1.919(2) . yes Mn N3 1.913(2) . yes Mn N1 1.923(2) . yes Mn O 2.0747(19) . yes P O 1.5015(19) . yes P C38 1.783(3) . ? P C44 1.790(3) . ? P C50 1.802(3) . ? F1 C21 1.345(3) . ? F2 C22 1.333(3) . ? F3 C23 1.340(3) . ? F4 C24 1.347(3) . ? F5 C25 1.347(3) . ? F6 C27 1.339(3) . ? F7 C28 1.346(3) . ? F8 C29 1.349(3) . ? F9 C30 1.342(3) . ? F10 C31 1.337(3) . ? F11 C33 1.342(3) . ? F12 C34 1.348(3) . ? F13 C35 1.340(3) . ? F14 C36 1.351(3) . ? F15 C37 1.361(3) . ? N1 C4 1.380(3) . ? N1 C1 1.391(3) . ? N2 C6 1.387(3) . ? N2 C9 1.393(3) . ? N3 C11 1.364(3) . ? N3 C14 1.374(3) . ? N4 C18 1.357(3) . ? N4 C15 1.378(4) . ? C1 C19 1.401(4) . ? C1 C2 1.421(4) . ? C2 C3 1.352(4) . ? C3 C4 1.424(4) . ? C4 C5 1.409(4) . ? C5 C6 1.404(4) . ? C5 C26 1.491(4) . ? C6 C7 1.435(4) . ? C7 C8 1.363(4) . ? C8 C9 1.431(4) . ? C9 C10 1.404(4) . ? C10 C11 1.416(4) . ? C10 C32 1.483(4) . ? C11 C12 1.425(4) . ? C12 C13 1.382(4) . ? C13 C14 1.416(4) . ? C14 C15 1.414(4) . ? C15 C16 1.421(4) . ? C16 C17 1.358(4) . ? C17 C18 1.438(4) . ? C18 C19 1.412(4) . ? C19 C20 1.499(4) . ? C20 C25 1.381(4) . ? C20 C21 1.374(4) . ? C21 C22 1.391(4) . ? C22 C23 1.378(4) . ? C23 C24 1.362(4) . ? C24 C25 1.378(4) . ? C26 C27 1.380(4) . ? C26 C31 1.399(4) . ? C27 C28 1.372(4) . ? C28 C29 1.384(4) . ? C29 C30 1.369(4) . ? C30 C31 1.370(4) . ? C32 C37 1.377(4) . ? C32 C33 1.407(4) . ? C33 C34 1.367(4) . ? C34 C35 1.373(4) . ? C35 C36 1.377(4) . ? C36 C37 1.366(4) . ? C38 C43 1.385(4) . ? C38 C39 1.392(5) . ? C39 C40 1.399(5) . ? C40 C41 1.377(5) . ? C41 C42 1.383(5) . ? C42 C43 1.383(5) . ? C44 C45 1.392(4) . ? C44 C49 1.405(4) . ? C45 C46 1.389(4) . ? C46 C47 1.391(5) . ? C47 C48 1.372(5) . ? C48 C49 1.385(4) . ? C50 C55 1.384(4) . ? C50 C51 1.398(4) . ? C51 C52 1.375(4) . ? C52 C53 1.367(5) . ? C53 C54 1.380(5) . ? C54 C55 1.395(5) . ? 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 N4 Mn N2 162.50(10) . . yes N4 Mn N3 80.31(10) . . yes N2 Mn N3 89.50(10) . . yes N4 Mn N1 89.26(10) . . yes N2 Mn N1 95.79(10) . . yes N3 Mn N1 159.52(10) . . yes N4 Mn O 96.60(9) . . yes N2 Mn O 98.68(9) . . yes N3 Mn O 96.56(9) . . yes N1 Mn O 102.14(9) . . yes O P C38 113.70(13) . . ? O P C44 111.31(13) . . ? C38 P C44 105.59(14) . . ? O P C50 108.02(13) . . ? C38 P C50 109.30(15) . . ? C44 P C50 108.84(14) . . ? P O Mn 158.61(13) . . yes C4 N1 C1 108.0(2) . . ? C4 N1 Mn 124.28(19) . . ? C1 N1 Mn 127.13(19) . . ? C6 N2 C9 108.0(2) . . ? C6 N2 Mn 124.73(19) . . ? C9 N2 Mn 126.73(19) . . ? C11 N3 C14 109.7(2) . . ? C11 N3 Mn 130.00(19) . . ? C14 N3 Mn 116.1(2) . . ? C18 N4 C15 110.0(2) . . ? C18 N4 Mn 133.1(2) . . ? C15 N4 Mn 116.7(2) . . ? N1 C1 C19 124.4(3) . . ? N1 C1 C2 107.3(3) . . ? C19 C1 C2 128.3(3) . . ? C3 C2 C1 108.9(3) . . ? C2 C3 C4 107.6(3) . . ? N1 C4 C5 123.9(3) . . ? N1 C4 C3 108.3(3) . . ? C5 C4 C3 127.8(3) . . ? C6 C5 C4 126.6(3) . . ? C6 C5 C26 117.7(3) . . ? C4 C5 C26 115.7(3) . . ? N2 C6 C5 123.5(3) . . ? N2 C6 C7 108.1(3) . . ? C5 C6 C7 128.3(3) . . ? C8 C7 C6 107.7(3) . . ? C7 C8 C9 108.3(3) . . ? C10 C9 N2 124.0(3) . . ? C10 C9 C8 128.2(3) . . ? N2 C9 C8 107.8(3) . . ? C9 C10 C11 124.1(3) . . ? C9 C10 C32 120.1(3) . . ? C11 C10 C32 115.8(3) . . ? N3 C11 C10 120.3(3) . . ? N3 C11 C12 107.4(3) . . ? C10 C11 C12 132.2(3) . . ? C13 C12 C11 107.7(3) . . ? C12 C13 C14 107.4(3) . . ? N3 C14 C15 112.5(3) . . ? N3 C14 C13 107.8(3) . . ? C15 C14 C13 139.4(3) . . ? N4 C15 C14 112.2(3) . . ? N4 C15 C16 107.1(3) . . ? C14 C15 C16 140.6(3) . . ? C17 C16 C15 108.0(3) . . ? C16 C17 C18 107.9(3) . . ? N4 C18 C19 120.0(3) . . ? N4 C18 C17 106.9(3) . . ? C19 C18 C17 132.9(3) . . ? C1 C19 C18 124.1(3) . . ? C1 C19 C20 118.3(3) . . ? C18 C19 C20 117.6(3) . . ? C25 C20 C21 116.3(3) . . ? C25 C20 C19 121.4(3) . . ? C21 C20 C19 122.2(3) . . ? F1 C21 C20 120.8(3) . . ? F1 C21 C22 116.8(3) . . ? C20 C21 C22 122.4(3) . . ? F2 C22 C23 120.2(3) . . ? F2 C22 C21 120.8(3) . . ? C23 C22 C21 119.0(3) . . ? F3 C23 C24 120.1(3) . . ? F3 C23 C22 119.9(3) . . ? C24 C23 C22 119.9(3) . . ? F4 C24 C23 120.3(3) . . ? F4 C24 C25 120.0(3) . . ? C23 C24 C25 119.8(3) . . ? F5 C25 C20 120.1(3) . . ? F5 C25 C24 117.4(3) . . ? C20 C25 C24 122.5(3) . . ? C27 C26 C31 116.0(3) . . ? C27 C26 C5 122.4(3) . . ? C31 C26 C5 121.4(3) . . ? F6 C27 C26 119.4(3) . . ? F6 C27 C28 117.8(3) . . ? C26 C27 C28 122.8(3) . . ? F7 C28 C27 121.3(3) . . ? F7 C28 C29 119.6(3) . . ? C27 C28 C29 119.1(3) . . ? F8 C29 C30 120.4(3) . . ? F8 C29 C28 119.3(3) . . ? C30 C29 C28 120.3(3) . . ? F9 C30 C29 119.2(3) . . ? F9 C30 C31 121.5(3) . . ? C29 C30 C31 119.3(3) . . ? F10 C31 C30 118.4(3) . . ? F10 C31 C26 119.1(3) . . ? C30 C31 C26 122.5(3) . . ? C37 C32 C33 115.1(3) . . ? C37 C32 C10 122.8(3) . . ? C33 C32 C10 121.7(3) . . ? F11 C33 C34 118.3(3) . . ? F11 C33 C32 119.4(3) . . ? C34 C33 C32 122.3(3) . . ? F12 C34 C33 120.3(3) . . ? F12 C34 C35 119.4(3) . . ? C33 C34 C35 120.3(3) . . ? F13 C35 C34 120.6(3) . . ? F13 C35 C36 120.3(3) . . ? C34 C35 C36 119.0(3) . . ? F14 C36 C37 120.3(3) . . ? F14 C36 C35 119.9(3) . . ? C37 C36 C35 119.8(3) . . ? F15 C37 C36 117.2(3) . . ? F15 C37 C32 119.3(3) . . ? C36 C37 C32 123.5(3) . . ? C43 C38 C39 119.2(3) . . ? C43 C38 P 118.9(3) . . ? C39 C38 P 121.7(3) . . ? C38 C39 C40 119.3(4) . . ? C41 C40 C39 120.5(4) . . ? C40 C41 C42 120.3(4) . . ? C43 C42 C41 119.3(4) . . ? C38 C43 C42 121.3(4) . . ? C45 C44 C49 119.0(3) . . ? C45 C44 P 118.7(2) . . ? C49 C44 P 122.3(3) . . ? C44 C45 C46 120.7(3) . . ? C45 C46 C47 119.6(4) . . ? C48 C47 C46 120.2(4) . . ? C47 C48 C49 120.9(3) . . ? C48 C49 C44 119.6(3) . . ? C55 C50 C51 119.6(3) . . ? C55 C50 P 118.1(2) . . ? C51 C50 P 122.3(2) . . ? C52 C51 C50 119.8(3) . . ? C51 C52 C53 121.1(4) . . ? C52 C53 C54 119.6(4) . . ? C53 C54 C55 120.6(4) . . ? C50 C55 C54 119.4(3) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.60 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.308 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.073