Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_address 'Qin, C. J.' ; Department of Chemistry 5735 South Ellis Ave. The University of Chicago, Chicago, IL 60637 USA ; 'Gavrilova, A.L.' ; Department of Chemistry 5735 South Ellis Ave. The University of Chicago, Chicago, IL 60637 USA ; 'Bosnich, B.' ; Department of Chemistry 5735 South Ellis Ave. The University of Chicago, Chicago, IL 60637 USA ; 'Incarvito, C. D.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 ; 'Lam, M.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 ; 'Rhatigan, B.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 ; 'Rheingold, A. L.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Brice Bosnich' _publ_contact_author_address ; Department of Chemistry University of Chicago 5735 South Ellis Avenue Chicago IL 60637 USA ; _publ_contact_author_phone '+773 702 0287' _publ_contact_author_fax '+773 702 0805' _publ_contact_author_email bos5@midway.uchicago.edu _publ_requested_journal 'Dalton Transactions' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Bimetallic Reactivity. Preparations, Properties and Structures of C omplexes Formed by Unsymmetrical Binucleating Ligands Bearing 4- and 6-Coordinate Sites Supported by Alkoxide Bridges ; # 3. Results data_complex_6 _database_code_CSD 170793 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 Cu2 F6 N5 O4 P' _chemical_formula_weight 852.74 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.0761(2) _cell_length_b 21.1395(2) _cell_length_c 19.3919(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.9872(2) _cell_angle_gamma 90.00 _cell_volume 7338.14(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rod _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.6289 _exptl_absorpt_correction_T_max 0.9047 _exptl_absorpt_process_details ? _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 '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 28593 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12168 _reflns_number_gt 10206 _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^)+(0.1000P)^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 12168 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 1.356 _refine_ls_restrained_S_all 1.356 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.86079(2) 0.42851(2) 0.75284(3) 0.02331(15) Uani 1 1 d . . . Cu2 Cu 0.99785(2) 0.343540(19) 0.80823(2) 0.01918(14) Uani 1 1 d . . . Cu3 Cu 0.36670(2) 0.42888(2) 0.73325(2) 0.02045(14) Uani 1 1 d . . . Cu4 Cu 0.50153(2) 0.342372(19) 0.78973(2) 0.01891(14) Uani 1 1 d . . . O1 O 0.79249(15) 0.44108(13) 0.67005(15) 0.0308(6) Uani 1 1 d . . . O2 O 0.93723(13) 0.41467(11) 0.83139(13) 0.0212(5) Uani 1 1 d . . . O3 O 0.91842(13) 0.28114(11) 0.81386(14) 0.0250(6) Uani 1 1 d . . . O4 O 0.81641(14) 0.33648(12) 0.76767(16) 0.0297(7) Uani 1 1 d . . . N1 N 0.83078(17) 0.50771(14) 0.79721(17) 0.0246(7) Uani 1 1 d . . . N2 N 1.04500(17) 0.36304(15) 0.92822(17) 0.0274(7) Uani 1 1 d . . . N3 N 1.08310(16) 0.40637(14) 0.79245(18) 0.0244(7) Uani 1 1 d . . . N4 N 1.05566(16) 0.28413(14) 0.75519(17) 0.0217(7) Uani 1 1 d . . . N5 N 0.94132(17) 0.39469(14) 0.68141(17) 0.0239(7) Uani 1 1 d . . . C1 C 0.74441(19) 0.48755(17) 0.6553(2) 0.0241(8) Uani 1 1 d . . . C2 C 0.7000(2) 0.48874(18) 0.5889(2) 0.0281(9) Uani 1 1 d . . . H2A H 0.7071 0.4567 0.5561 0.034 Uiso 1 1 calc R . . C3 C 0.6467(2) 0.53506(19) 0.5703(2) 0.0326(9) Uani 1 1 d . . . H3A H 0.6187 0.5346 0.5251 0.039 Uiso 1 1 calc R . . C4 C 0.6336(2) 0.5827(2) 0.6177(2) 0.0362(10) Uani 1 1 d . . . H4A H 0.5956 0.6134 0.6057 0.043 Uiso 1 1 calc R . . C5 C 0.6775(2) 0.58389(19) 0.6826(2) 0.0329(10) Uani 1 1 d . . . H5A H 0.6701 0.6167 0.7144 0.040 Uiso 1 1 calc R . . C6 C 0.7333(2) 0.53744(17) 0.7029(2) 0.0235(8) Uani 1 1 d . . . C7 C 0.7772(2) 0.54437(17) 0.7700(2) 0.0262(8) Uani 1 1 d . . . H7A H 0.7657 0.5794 0.7973 0.031 Uiso 1 1 calc R . . C8 C 0.8689(2) 0.52152(18) 0.8681(2) 0.0294(9) Uani 1 1 d . . . H8A H 0.8445 0.5580 0.8877 0.035 Uiso 1 1 calc R . . H8B H 0.9216 0.5328 0.8659 0.035 Uiso 1 1 calc R . . C9 C 0.8656(2) 0.46383(18) 0.9152(2) 0.0281(9) Uani 1 1 d . . . H9A H 0.8137 0.4478 0.9094 0.034 Uiso 1 1 calc R . . H9B H 0.8785 0.4774 0.9643 0.034 Uiso 1 1 calc R . . C10 C 0.9181(2) 0.40921(18) 0.9010(2) 0.0283(9) Uani 1 1 d . . . H10A H 0.8927 0.3678 0.9060 0.034 Uiso 1 1 calc R . . C11 C 0.9916(2) 0.41097(19) 0.9500(2) 0.0318(9) Uani 1 1 d . . . H11A H 1.0139 0.4537 0.9494 0.038 Uiso 1 1 calc R . . H11B H 0.9822 0.4019 0.9981 0.038 Uiso 1 1 calc R . . C12 C 1.0554(2) 0.3101(2) 0.9797(2) 0.0336(10) Uani 1 1 d . . . H12A H 1.0057 0.2976 0.9910 0.040 Uiso 1 1 calc R . . H12B H 1.0849 0.3261 1.0230 0.040 Uiso 1 1 calc R . . C13 C 1.0938(2) 0.25183(18) 0.9563(2) 0.0293(9) Uani 1 1 d . . . C14 C 1.1680(2) 0.2368(2) 0.9857(3) 0.0390(11) Uani 1 1 d . . . H14A H 1.1949 0.2646 1.0186 0.047 Uiso 1 1 calc R . . C15 C 1.2012(3) 0.1813(2) 0.9664(3) 0.0444(12) Uani 1 1 d . . . H15A H 1.2512 0.1717 0.9857 0.053 Uiso 1 1 calc R . . C16 C 1.1620(3) 0.1399(2) 0.9194(3) 0.0445(12) Uani 1 1 d . . . H16A H 1.1848 0.1019 0.9068 0.053 Uiso 1 1 calc R . . C17 C 1.0892(3) 0.1544(2) 0.8907(3) 0.0452(12) Uani 1 1 d . . . H17A H 1.0622 0.1263 0.8581 0.054 Uiso 1 1 calc R . . C18 C 1.0556(3) 0.2098(2) 0.9097(2) 0.0374(10) Uani 1 1 d . . . H18A H 1.0055 0.2189 0.8902 0.045 Uiso 1 1 calc R . . C19 C 1.1181(2) 0.39311(19) 0.9209(2) 0.0325(10) Uani 1 1 d . . . H19A H 1.1548 0.3599 0.9136 0.039 Uiso 1 1 calc R . . H19B H 1.1370 0.4159 0.9644 0.039 Uiso 1 1 calc R . . C20 C 1.1108(2) 0.43924(18) 0.8600(2) 0.0307(9) Uani 1 1 d . . . H20A H 1.0756 0.4734 0.8682 0.037 Uiso 1 1 calc R . . H20B H 1.1600 0.4587 0.8569 0.037 Uiso 1 1 calc R . . C21 C 1.14552(19) 0.37060(18) 0.7671(2) 0.0279(9) Uani 1 1 d . . . H21A H 1.1866 0.3651 0.8060 0.033 Uiso 1 1 calc R . . H21B H 1.1650 0.3955 0.7303 0.033 Uiso 1 1 calc R . . C22 C 1.12079(19) 0.30634(18) 0.7383(2) 0.0239(8) Uani 1 1 d . . . C23 C 1.1638(2) 0.2717(2) 0.6977(2) 0.0306(9) Uani 1 1 d . . . H23A H 1.2088 0.2888 0.6854 0.037 Uiso 1 1 calc R . . C24 C 1.1402(2) 0.2114(2) 0.6752(2) 0.0335(10) Uani 1 1 d . . . H24A H 1.1697 0.1862 0.6489 0.040 Uiso 1 1 calc R . . C25 C 1.0724(2) 0.18904(19) 0.6920(2) 0.0355(10) Uani 1 1 d . . . H25A H 1.0543 0.1486 0.6761 0.043 Uiso 1 1 calc R . . C26 C 1.0318(2) 0.22585(17) 0.7316(2) 0.0281(9) Uani 1 1 d . . . H26A H 0.9857 0.2102 0.7428 0.034 Uiso 1 1 calc R . . C27 C 1.0485(2) 0.45371(17) 0.7386(2) 0.0263(9) Uani 1 1 d . . . H27A H 1.0121 0.4805 0.7588 0.032 Uiso 1 1 calc R . . H27B H 1.0879 0.4815 0.7245 0.032 Uiso 1 1 calc R . . C28 C 1.0096(2) 0.41909(17) 0.6756(2) 0.0241(8) Uani 1 1 d . . . C29 C 1.0450(2) 0.4083(2) 0.6171(2) 0.0345(10) Uani 1 1 d . . . H29A H 1.0914 0.4278 0.6129 0.041 Uiso 1 1 calc R . . C30 C 1.0109(3) 0.3682(2) 0.5650(2) 0.0400(11) Uani 1 1 d . . . H30A H 1.0340 0.3600 0.5249 0.048 Uiso 1 1 calc R . . C31 C 0.9430(2) 0.34068(19) 0.5724(2) 0.0348(10) Uani 1 1 d . . . H31A H 0.9199 0.3118 0.5385 0.042 Uiso 1 1 calc R . . C32 C 0.9092(2) 0.35581(18) 0.6301(2) 0.0265(8) Uani 1 1 d . . . H32A H 0.8615 0.3383 0.6339 0.032 Uiso 1 1 calc R . . C33 C 0.8478(2) 0.28939(18) 0.7987(2) 0.0290(9) Uani 1 1 d . . . C34 C 0.7992(2) 0.2376(2) 0.8214(3) 0.0491(14) Uani 1 1 d . . . H34A H 0.7465 0.2484 0.8074 0.074 Uiso 1 1 calc R . . H34B H 0.8090 0.2330 0.8722 0.074 Uiso 1 1 calc R . . H34C H 0.8105 0.1977 0.7994 0.074 Uiso 1 1 calc R . . P1 P 0.33606(6) 0.38578(5) 0.06847(6) 0.0339(3) Uani 1 1 d . . . F1 F 0.3598(3) 0.3164(2) 0.0786(4) 0.149(2) Uani 1 1 d . . . F2 F 0.30977(19) 0.3736(3) -0.01124(19) 0.1055(16) Uani 1 1 d . . . F3 F 0.3111(2) 0.45603(17) 0.0605(4) 0.151(3) Uani 1 1 d . . . F4 F 0.3619(2) 0.3986(3) 0.1489(2) 0.1096(17) Uani 1 1 d . . . F5 F 0.41715(18) 0.4057(2) 0.0535(2) 0.0933(13) Uani 1 1 d . . . F6 F 0.25294(17) 0.36840(17) 0.08232(18) 0.0664(9) Uani 1 1 d . . . O1' O 0.30044(15) 0.43932(13) 0.64885(15) 0.0318(7) Uani 1 1 d . . . O2' O 0.45104(13) 0.42218(11) 0.80688(13) 0.0204(5) Uani 1 1 d . . . O3' O 0.42384(13) 0.28851(11) 0.81999(15) 0.0250(6) Uani 1 1 d . . . O4' O 0.32011(14) 0.33739(12) 0.76753(15) 0.0263(6) Uani 1 1 d . . . N1' N 0.30808(16) 0.48816(14) 0.78533(16) 0.0230(7) Uani 1 1 d . . . N2' N 0.56496(17) 0.36912(14) 0.90030(17) 0.0251(7) Uani 1 1 d . . . N3' N 0.58841(16) 0.39278(14) 0.75630(17) 0.0237(7) Uani 1 1 d . . . N4' N 0.54090(16) 0.27190(14) 0.73475(17) 0.0233(7) Uani 1 1 d . . . N5' N 0.43492(16) 0.38312(15) 0.66186(17) 0.0232(7) Uani 1 1 d . . . C1' C 0.2482(2) 0.48216(17) 0.6325(2) 0.0235(8) Uani 1 1 d . . . C2' C 0.2120(2) 0.48609(18) 0.5628(2) 0.0267(8) Uani 1 1 d . . . H2'A H 0.2264 0.4579 0.5289 0.032 Uiso 1 1 calc R . . C3' C 0.1560(2) 0.53021(19) 0.5430(2) 0.0320(9) Uani 1 1 d . . . H3'A H 0.1334 0.5321 0.4958 0.038 Uiso 1 1 calc R . . C4' C 0.1323(2) 0.57211(19) 0.5921(2) 0.0342(10) Uani 1 1 d . . . H4'A H 0.0935 0.6017 0.5786 0.041 Uiso 1 1 calc R . . C5' C 0.1666(2) 0.56941(18) 0.6601(2) 0.0309(9) Uani 1 1 d . . . H5'A H 0.1510 0.5978 0.6932 0.037 Uiso 1 1 calc R . . C6' C 0.2244(2) 0.52540(17) 0.6822(2) 0.0237(8) Uani 1 1 d . . . C7' C 0.2548(2) 0.52427(16) 0.7548(2) 0.0231(8) Uani 1 1 d . . . H7'A H 0.2336 0.5532 0.7840 0.028 Uiso 1 1 calc R . . C8' C 0.3211(2) 0.48981(19) 0.8622(2) 0.0292(9) Uani 1 1 d . . . H8'A H 0.2969 0.4525 0.8804 0.035 Uiso 1 1 calc R . . H8'B H 0.2972 0.5282 0.8784 0.035 Uiso 1 1 calc R . . C9' C 0.4040(2) 0.48999(17) 0.8925(2) 0.0283(9) Uani 1 1 d . . . H9'A H 0.4290 0.5256 0.8721 0.034 Uiso 1 1 calc R . . H9'B H 0.4086 0.4970 0.9434 0.034 Uiso 1 1 calc R . . C10' C 0.4437(2) 0.42837(17) 0.8786(2) 0.0242(8) Uani 1 1 d . . . H10B H 0.4133 0.3921 0.8923 0.029 Uiso 1 1 calc R . . C11' C 0.5212(2) 0.42521(18) 0.9214(2) 0.0286(9) Uani 1 1 d . . . H11C H 0.5488 0.4647 0.9146 0.034 Uiso 1 1 calc R . . H11D H 0.5161 0.4218 0.9715 0.034 Uiso 1 1 calc R . . C12' C 0.5730(2) 0.32225(19) 0.9583(2) 0.0321(9) Uani 1 1 d . . . H12C H 0.5227 0.3134 0.9707 0.038 Uiso 1 1 calc R . . H12D H 0.6027 0.3420 0.9994 0.038 Uiso 1 1 calc R . . C13' C 0.6091(2) 0.25979(18) 0.9441(2) 0.0284(9) Uani 1 1 d . . . C14' C 0.6784(2) 0.2432(2) 0.9820(2) 0.0383(10) Uani 1 1 d . . . H14B H 0.7040 0.2725 1.0140 0.046 Uiso 1 1 calc R . . C15' C 0.7100(3) 0.1839(2) 0.9728(3) 0.0490(13) Uani 1 1 d . . . H15B H 0.7564 0.1728 0.9994 0.059 Uiso 1 1 calc R . . C16' C 0.6742(3) 0.1414(2) 0.9256(3) 0.0462(12) Uani 1 1 d . . . H16B H 0.6962 0.1013 0.9193 0.055 Uiso 1 1 calc R . . C17' C 0.6061(3) 0.1570(2) 0.8870(3) 0.0417(11) Uani 1 1 d . . . H17B H 0.5816 0.1278 0.8542 0.050 Uiso 1 1 calc R . . C18' C 0.5732(2) 0.21626(18) 0.8969(2) 0.0284(9) Uani 1 1 d . . . H18B H 0.5262 0.2266 0.8710 0.034 Uiso 1 1 calc R . . C19' C 0.6385(2) 0.38972(19) 0.8829(2) 0.0300(9) Uani 1 1 d . . . H19C H 0.6694 0.3521 0.8763 0.036 Uiso 1 1 calc R . . H19D H 0.6648 0.4148 0.9220 0.036 Uiso 1 1 calc R . . C20' C 0.6289(2) 0.42972(18) 0.8164(2) 0.0296(9) Uani 1 1 d . . . H20C H 0.6004 0.4685 0.8239 0.035 Uiso 1 1 calc R . . H20D H 0.6786 0.4427 0.8054 0.035 Uiso 1 1 calc R . . C21' C 0.6406(2) 0.34845(18) 0.7280(2) 0.0294(9) Uani 1 1 d . . . H21C H 0.6857 0.3429 0.7628 0.035 Uiso 1 1 calc R . . H21D H 0.6565 0.3671 0.6856 0.035 Uiso 1 1 calc R . . C22' C 0.6055(2) 0.28408(19) 0.7102(2) 0.0266(8) Uani 1 1 d . . . C23' C 0.6406(2) 0.2391(2) 0.6731(2) 0.0384(11) Uani 1 1 d . . . H23B H 0.6867 0.2484 0.6570 0.046 Uiso 1 1 calc R . . C24' C 0.6067(2) 0.1803(2) 0.6604(2) 0.0418(11) Uani 1 1 d . . . H24B H 0.6301 0.1483 0.6366 0.050 Uiso 1 1 calc R . . C25' C 0.5380(2) 0.1691(2) 0.6831(3) 0.0405(11) Uani 1 1 d . . . H25B H 0.5127 0.1302 0.6728 0.049 Uiso 1 1 calc R . . C26' C 0.5075(2) 0.21506(19) 0.7203(2) 0.0303(9) Uani 1 1 d . . . H26B H 0.4612 0.2068 0.7367 0.036 Uiso 1 1 calc R . . C27' C 0.5528(2) 0.43840(18) 0.7005(2) 0.0271(9) Uani 1 1 d . . . H27C H 0.5233 0.4707 0.7216 0.033 Uiso 1 1 calc R . . H27D H 0.5921 0.4603 0.6787 0.033 Uiso 1 1 calc R . . C28' C 0.5024(2) 0.40137(17) 0.6457(2) 0.0233(8) Uani 1 1 d . . . C29' C 0.5273(2) 0.3822(2) 0.5841(2) 0.0363(10) Uani 1 1 d . . . H29B H 0.5731 0.3978 0.5721 0.044 Uiso 1 1 calc R . . C30' C 0.4846(3) 0.3400(2) 0.5406(2) 0.0419(11) Uani 1 1 d . . . H30B H 0.5011 0.3261 0.4987 0.050 Uiso 1 1 calc R . . C31' C 0.4179(2) 0.3184(2) 0.5586(2) 0.0352(10) Uani 1 1 d . . . H31B H 0.3888 0.2882 0.5305 0.042 Uiso 1 1 calc R . . C32' C 0.3944(2) 0.34148(18) 0.6185(2) 0.0273(9) Uani 1 1 d . . . H32B H 0.3477 0.3276 0.6300 0.033 Uiso 1 1 calc R . . C33' C 0.35302(19) 0.29829(17) 0.8100(2) 0.0223(8) Uani 1 1 d . . . C34' C 0.3079(2) 0.25977(19) 0.8550(2) 0.0335(10) Uani 1 1 d . . . H34D H 0.2549 0.2706 0.8436 0.050 Uiso 1 1 calc R . . H34E H 0.3246 0.2691 0.9042 0.050 Uiso 1 1 calc R . . H34F H 0.3148 0.2146 0.8463 0.050 Uiso 1 1 calc R . . P1' P 0.15339(7) 0.64889(6) 0.89854(7) 0.0403(3) Uani 1 1 d . . . F1' F 0.1421(3) 0.57727(17) 0.9125(2) 0.1160(18) Uani 1 1 d . . . F2' F 0.1314(2) 0.6378(3) 0.81658(18) 0.1035(15) Uani 1 1 d . . . F3' F 0.17456(19) 0.65936(16) 0.98055(18) 0.0696(10) Uani 1 1 d . . . F4' F 0.1731(3) 0.72219(17) 0.8879(2) 0.1116(17) Uani 1 1 d . . . F5' F 0.23900(17) 0.63636(19) 0.8911(2) 0.0789(11) Uani 1 1 d . . . F6' F 0.07091(19) 0.6661(3) 0.9055(2) 0.124(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 Cu1 0.0215(3) 0.0230(3) 0.0246(3) -0.00225(18) 0.0005(2) 0.00688(17) Cu2 0.0161(2) 0.0166(2) 0.0250(3) -0.00264(16) 0.00331(19) 0.00176(16) Cu3 0.0187(2) 0.0223(2) 0.0200(3) -0.00207(17) 0.00158(19) 0.00237(17) Cu4 0.0150(2) 0.0192(2) 0.0228(3) -0.00035(16) 0.00369(18) -0.00111(16) O1 0.0281(15) 0.0322(15) 0.0300(17) -0.0029(12) -0.0038(12) 0.0096(12) O2 0.0239(13) 0.0194(12) 0.0211(15) 0.0002(10) 0.0060(11) 0.0055(10) O3 0.0195(13) 0.0212(13) 0.0339(17) 0.0015(11) 0.0021(11) 0.0018(10) O4 0.0200(13) 0.0261(14) 0.0424(19) 0.0087(12) 0.0021(12) -0.0024(11) N1 0.0260(16) 0.0226(16) 0.0245(19) -0.0009(13) 0.0015(14) 0.0007(13) N2 0.0265(17) 0.0287(17) 0.026(2) -0.0012(14) -0.0012(14) 0.0102(14) N3 0.0200(15) 0.0186(15) 0.035(2) -0.0067(13) 0.0067(14) 0.0000(12) N4 0.0233(16) 0.0217(15) 0.0203(18) 0.0005(12) 0.0033(13) 0.0029(12) N5 0.0226(16) 0.0227(16) 0.0268(19) 0.0011(13) 0.0048(13) 0.0029(12) C1 0.0181(17) 0.0236(19) 0.031(2) 0.0082(16) 0.0057(16) -0.0016(14) C2 0.027(2) 0.031(2) 0.025(2) 0.0040(16) 0.0032(17) -0.0019(16) C3 0.035(2) 0.032(2) 0.029(3) 0.0101(17) 0.0004(18) -0.0007(18) C4 0.037(2) 0.033(2) 0.037(3) 0.0133(19) 0.001(2) 0.0099(18) C5 0.036(2) 0.025(2) 0.038(3) 0.0047(17) 0.0060(19) 0.0083(17) C6 0.0235(18) 0.0207(18) 0.026(2) 0.0060(15) 0.0040(16) 0.0004(15) C7 0.029(2) 0.0173(18) 0.033(2) 0.0020(15) 0.0063(17) 0.0040(15) C8 0.031(2) 0.0236(19) 0.032(2) -0.0080(16) 0.0004(17) 0.0055(16) C9 0.028(2) 0.032(2) 0.024(2) -0.0022(16) 0.0034(16) 0.0095(16) C10 0.033(2) 0.027(2) 0.025(2) -0.0035(16) 0.0050(17) 0.0077(16) C11 0.036(2) 0.034(2) 0.026(2) -0.0087(17) 0.0036(18) 0.0081(18) C12 0.042(2) 0.042(2) 0.017(2) 0.0038(17) 0.0043(17) 0.0164(19) C13 0.037(2) 0.032(2) 0.020(2) 0.0074(16) 0.0059(17) 0.0090(17) C14 0.033(2) 0.039(2) 0.044(3) 0.007(2) 0.004(2) 0.0057(19) C15 0.036(2) 0.042(3) 0.057(3) 0.012(2) 0.013(2) 0.012(2) C16 0.063(3) 0.030(2) 0.045(3) 0.010(2) 0.021(2) 0.020(2) C17 0.070(3) 0.034(2) 0.029(3) 0.0006(18) -0.001(2) 0.009(2) C18 0.046(3) 0.036(2) 0.029(3) 0.0076(18) 0.000(2) 0.0126(19) C19 0.026(2) 0.034(2) 0.034(3) -0.0111(18) -0.0083(18) 0.0038(17) C20 0.0219(19) 0.027(2) 0.042(3) -0.0104(17) -0.0027(18) -0.0038(16) C21 0.0153(17) 0.028(2) 0.041(3) -0.0058(17) 0.0045(16) 0.0010(15) C22 0.0183(18) 0.027(2) 0.025(2) -0.0023(15) -0.0003(15) 0.0050(15) C23 0.0193(19) 0.043(2) 0.030(2) -0.0055(18) 0.0058(17) 0.0049(17) C24 0.033(2) 0.042(2) 0.025(2) -0.0083(17) 0.0001(17) 0.0160(18) C25 0.039(2) 0.027(2) 0.039(3) -0.0101(18) -0.0002(19) 0.0046(18) C26 0.031(2) 0.0221(19) 0.031(2) -0.0038(16) 0.0031(17) 0.0001(16) C27 0.0194(18) 0.0227(19) 0.037(3) 0.0059(16) 0.0049(16) -0.0044(15) C28 0.0212(18) 0.0212(18) 0.030(2) 0.0071(15) 0.0047(16) 0.0025(14) C29 0.028(2) 0.043(2) 0.034(3) 0.0082(19) 0.0118(18) -0.0007(18) C30 0.045(3) 0.049(3) 0.028(3) -0.002(2) 0.013(2) 0.015(2) C31 0.042(2) 0.036(2) 0.026(3) -0.0030(17) 0.0034(19) 0.0112(19) C32 0.030(2) 0.0251(19) 0.024(2) 0.0008(16) 0.0014(16) 0.0026(16) C33 0.0209(19) 0.024(2) 0.043(3) 0.0042(17) 0.0066(17) 0.0014(15) C34 0.031(2) 0.038(3) 0.079(4) 0.028(2) 0.009(2) -0.0025(19) P1 0.0320(6) 0.0362(6) 0.0355(7) -0.0011(5) 0.0114(5) 0.0001(5) F1 0.139(4) 0.054(3) 0.248(7) 0.008(3) 0.001(4) 0.049(3) F2 0.063(2) 0.215(5) 0.040(2) -0.016(3) 0.0102(17) -0.030(3) F3 0.097(3) 0.039(2) 0.303(8) 0.020(3) -0.022(4) -0.003(2) F4 0.072(3) 0.213(5) 0.044(3) -0.035(3) 0.0108(19) -0.023(3) F5 0.0446(19) 0.171(4) 0.066(3) 0.008(2) 0.0151(17) -0.026(2) F6 0.0498(18) 0.088(2) 0.067(2) -0.0133(18) 0.0291(16) -0.0226(17) O1' 0.0300(15) 0.0382(16) 0.0249(17) -0.0055(12) -0.0043(12) 0.0144(12) O2' 0.0194(12) 0.0207(13) 0.0207(15) -0.0027(10) 0.0015(10) 0.0001(10) O3' 0.0183(13) 0.0211(13) 0.0360(17) -0.0004(11) 0.0047(11) -0.0013(10) O4' 0.0196(13) 0.0262(14) 0.0322(17) 0.0053(11) 0.0008(12) -0.0036(10) N1' 0.0247(16) 0.0234(16) 0.0211(18) -0.0031(12) 0.0038(13) 0.0019(13) N2' 0.0258(16) 0.0238(16) 0.0248(19) -0.0016(13) 0.0006(13) 0.0009(13) N3' 0.0140(14) 0.0261(16) 0.030(2) 0.0056(13) 0.0004(13) -0.0010(12) N4' 0.0207(15) 0.0256(16) 0.0242(19) -0.0031(13) 0.0048(13) 0.0011(13) N5' 0.0198(15) 0.0287(17) 0.0212(18) 0.0038(13) 0.0039(13) 0.0061(13) C1' 0.0217(18) 0.0238(19) 0.025(2) 0.0039(15) 0.0042(15) -0.0010(15) C2' 0.032(2) 0.029(2) 0.019(2) 0.0037(15) 0.0028(16) -0.0041(16) C3' 0.028(2) 0.036(2) 0.030(3) 0.0109(18) -0.0017(17) -0.0057(17) C4' 0.036(2) 0.027(2) 0.040(3) 0.0139(17) 0.004(2) 0.0090(17) C5' 0.036(2) 0.024(2) 0.033(3) 0.0078(16) 0.0068(19) 0.0021(16) C6' 0.0245(19) 0.0188(18) 0.029(2) 0.0032(15) 0.0062(16) 0.0019(15) C7' 0.0236(18) 0.0181(17) 0.028(2) -0.0010(14) 0.0049(16) 0.0001(14) C8' 0.036(2) 0.029(2) 0.023(2) 0.0024(16) 0.0054(17) 0.0075(17) C9' 0.037(2) 0.0224(19) 0.024(2) -0.0043(15) 0.0017(17) 0.0005(16) C10' 0.028(2) 0.0265(19) 0.019(2) -0.0023(14) 0.0055(16) -0.0025(15) C11' 0.031(2) 0.027(2) 0.026(2) -0.0065(15) -0.0011(17) -0.0008(16) C12' 0.036(2) 0.036(2) 0.024(2) 0.0025(17) 0.0063(18) 0.0034(18) C13' 0.030(2) 0.031(2) 0.025(2) 0.0095(16) 0.0070(17) 0.0037(16) C14' 0.032(2) 0.046(3) 0.036(3) 0.007(2) -0.0006(19) 0.0015(19) C15' 0.035(2) 0.051(3) 0.061(4) 0.019(3) 0.005(2) 0.016(2) C16' 0.051(3) 0.043(3) 0.047(3) 0.011(2) 0.015(2) 0.018(2) C17' 0.055(3) 0.035(2) 0.037(3) 0.0024(19) 0.011(2) 0.009(2) C18' 0.034(2) 0.031(2) 0.020(2) 0.0071(16) 0.0028(17) 0.0061(17) C19' 0.0234(19) 0.031(2) 0.032(2) 0.0008(17) -0.0085(17) -0.0056(16) C20' 0.0225(19) 0.029(2) 0.036(3) 0.0039(17) -0.0006(17) -0.0111(15) C21' 0.0168(18) 0.037(2) 0.035(3) 0.0081(17) 0.0042(17) 0.0039(16) C22' 0.0186(18) 0.038(2) 0.022(2) 0.0074(16) 0.0003(15) 0.0073(16) C23' 0.027(2) 0.059(3) 0.031(3) -0.002(2) 0.0127(18) 0.010(2) C24' 0.040(2) 0.050(3) 0.036(3) -0.017(2) 0.007(2) 0.014(2) C25' 0.041(3) 0.036(2) 0.042(3) -0.017(2) 0.000(2) 0.0005(19) C26' 0.025(2) 0.034(2) 0.032(3) -0.0045(17) 0.0037(17) 0.0020(16) C27' 0.025(2) 0.0259(19) 0.031(2) 0.0095(16) 0.0040(17) -0.0042(15) C28' 0.0248(19) 0.0268(19) 0.019(2) 0.0078(15) 0.0069(15) 0.0036(15) C29' 0.031(2) 0.049(3) 0.030(3) 0.011(2) 0.0113(19) 0.0104(19) C30' 0.048(3) 0.051(3) 0.029(3) 0.000(2) 0.012(2) 0.017(2) C31' 0.038(2) 0.034(2) 0.033(3) -0.0036(18) 0.0010(19) 0.0089(18) C32' 0.023(2) 0.033(2) 0.026(2) -0.0010(16) 0.0027(16) 0.0029(15) C33' 0.0183(18) 0.0235(18) 0.025(2) -0.0059(15) 0.0033(15) -0.0031(14) C34' 0.023(2) 0.034(2) 0.042(3) 0.0130(19) 0.0033(18) -0.0033(17) P1' 0.0425(7) 0.0434(7) 0.0383(8) 0.0025(5) 0.0176(6) 0.0113(5) F1' 0.197(5) 0.049(2) 0.105(4) -0.010(2) 0.032(3) -0.056(3) F2' 0.079(3) 0.199(5) 0.032(2) -0.015(2) 0.0078(18) 0.027(3) F3' 0.081(2) 0.083(2) 0.048(2) -0.0075(16) 0.0194(17) -0.0178(18) F4' 0.175(4) 0.047(2) 0.126(4) 0.030(2) 0.069(3) 0.037(2) F5' 0.0518(19) 0.089(2) 0.101(3) -0.018(2) 0.0292(19) 0.0026(18) F6' 0.044(2) 0.250(6) 0.076(3) -0.029(3) 0.0060(19) 0.041(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 Cu1 O1 1.903(3) . ? Cu1 O2 1.932(3) . ? Cu1 N1 1.992(3) . ? Cu1 O4 2.139(3) . ? Cu1 N5 2.260(3) . ? Cu2 O2 1.949(2) . ? Cu2 O3 1.964(2) . ? Cu2 N4 2.006(3) . ? Cu2 N3 2.089(3) . ? Cu2 N2 2.400(3) . ? Cu3 O1' 1.902(3) . ? Cu3 O2' 1.944(3) . ? Cu3 N1' 2.003(3) . ? Cu3 N5' 2.202(3) . ? Cu3 O4' 2.247(2) . ? Cu4 O3' 1.960(2) . ? Cu4 O2' 1.968(2) . ? Cu4 N4' 2.018(3) . ? Cu4 N3' 2.075(3) . ? Cu4 N2' 2.356(3) . ? O1 C1 1.316(4) . ? O2 C10 1.443(5) . ? O3 C33 1.282(4) . ? O4 C33 1.257(5) . ? N1 C7 1.294(5) . ? N1 C8 1.478(5) . ? N2 C19 1.491(5) . ? N2 C12 1.493(5) . ? N2 C11 1.500(5) . ? N3 C21 1.497(4) . ? N3 C20 1.506(5) . ? N3 C27 1.518(5) . ? N4 C22 1.349(5) . ? N4 C26 1.363(5) . ? N5 C28 1.356(5) . ? N5 C32 1.357(5) . ? C1 C2 1.419(6) . ? C1 C6 1.434(5) . ? C2 C3 1.387(5) . ? C3 C4 1.406(6) . ? C4 C5 1.392(6) . ? C5 C6 1.424(5) . ? C6 C7 1.434(5) . ? C8 C9 1.530(5) . ? C9 C10 1.544(5) . ? C10 C11 1.523(6) . ? C12 C13 1.515(5) . ? C13 C18 1.381(6) . ? C13 C14 1.418(6) . ? C14 C15 1.394(6) . ? C15 C16 1.385(7) . ? C16 C17 1.390(7) . ? C17 C18 1.394(6) . ? C19 C20 1.522(6) . ? C21 C22 1.512(5) . ? C22 C23 1.391(5) . ? C23 C24 1.393(6) . ? C24 C25 1.395(6) . ? C25 C26 1.375(6) . ? C27 C28 1.511(5) . ? C28 C29 1.396(6) . ? C29 C30 1.394(6) . ? C30 C31 1.384(6) . ? C31 C32 1.385(6) . ? C33 C34 1.507(5) . ? P1 F1 1.532(4) . ? P1 F3 1.554(4) . ? P1 F2 1.574(4) . ? P1 F4 1.588(4) . ? P1 F5 1.590(3) . ? P1 F6 1.605(3) . ? O1' C1' 1.315(4) . ? O2' C10' 1.422(5) . ? O3' C33' 1.285(4) . ? O4' C33' 1.257(5) . ? N1' C7' 1.305(5) . ? N1' C8' 1.477(5) . ? N2' C19' 1.482(5) . ? N2' C12' 1.490(5) . ? N2' C11' 1.513(5) . ? N3' C21' 1.487(5) . ? N3' C20' 1.506(5) . ? N3' C27' 1.524(5) . ? N4' C22' 1.346(5) . ? N4' C26' 1.357(5) . ? N5' C28' 1.357(5) . ? N5' C32' 1.358(5) . ? C1' C2' 1.421(5) . ? C1' C6' 1.436(5) . ? C2' C3' 1.390(5) . ? C3' C4' 1.410(6) . ? C4' C5' 1.377(6) . ? C5' C6' 1.420(5) . ? C6' C7' 1.440(5) . ? C8' C9' 1.531(5) . ? C9' C10' 1.529(5) . ? C10' C11' 1.527(5) . ? C12' C13' 1.515(5) . ? C13' C18' 1.393(6) . ? C13' C14' 1.406(6) . ? C14' C15' 1.399(7) . ? C15' C16' 1.379(8) . ? C16' C17' 1.389(7) . ? C17' C18' 1.411(6) . ? C19' C20' 1.532(6) . ? C21' C22' 1.521(6) . ? C22' C23' 1.396(6) . ? C23' C24' 1.392(6) . ? C24' C25' 1.394(6) . ? C25' C26' 1.372(6) . ? C27' C28' 1.517(5) . ? C28' C29' 1.393(6) . ? C29' C30' 1.387(6) . ? C30' C31' 1.378(6) . ? C31' C32' 1.380(6) . ? C33' C34' 1.512(5) . ? P1' F1' 1.556(4) . ? P1' F6' 1.559(3) . ? P1' F5' 1.596(3) . ? P1' F3' 1.598(4) . ? P1' F2' 1.601(4) . ? P1' F4' 1.609(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 O1 Cu1 O2 174.68(11) . . ? O1 Cu1 N1 93.64(12) . . ? O2 Cu1 N1 89.68(12) . . ? O1 Cu1 O4 91.66(12) . . ? O2 Cu1 O4 89.81(10) . . ? N1 Cu1 O4 125.22(12) . . ? O1 Cu1 N5 85.69(12) . . ? O2 Cu1 N5 89.10(11) . . ? N1 Cu1 N5 140.16(12) . . ? O4 Cu1 N5 94.60(11) . . ? O2 Cu2 O3 93.82(10) . . ? O2 Cu2 N4 161.87(12) . . ? O3 Cu2 N4 92.58(12) . . ? O2 Cu2 N3 89.60(11) . . ? O3 Cu2 N3 174.34(12) . . ? N4 Cu2 N3 82.85(12) . . ? O2 Cu2 N2 77.26(11) . . ? O3 Cu2 N2 103.03(12) . . ? N4 Cu2 N2 117.67(12) . . ? N3 Cu2 N2 82.13(13) . . ? O1' Cu3 O2' 167.55(12) . . ? O1' Cu3 N1' 92.71(12) . . ? O2' Cu3 N1' 95.23(11) . . ? O1' Cu3 N5' 81.42(11) . . ? O2' Cu3 N5' 88.81(11) . . ? N1' Cu3 N5' 166.88(12) . . ? O1' Cu3 O4' 97.90(11) . . ? O2' Cu3 O4' 90.45(10) . . ? N1' Cu3 O4' 98.23(11) . . ? N5' Cu3 O4' 94.22(11) . . ? O3' Cu4 O2' 94.53(10) . . ? O3' Cu4 N4' 92.82(12) . . ? O2' Cu4 N4' 158.09(12) . . ? O3' Cu4 N3' 175.39(11) . . ? O2' Cu4 N3' 90.08(11) . . ? N4' Cu4 N3' 82.90(12) . . ? O3' Cu4 N2' 98.36(11) . . ? O2' Cu4 N2' 79.57(10) . . ? N4' Cu4 N2' 119.69(12) . . ? N3' Cu4 N2' 82.37(12) . . ? C1 O1 Cu1 128.2(3) . . ? C10 O2 Cu1 120.8(2) . . ? C10 O2 Cu2 111.6(2) . . ? Cu1 O2 Cu2 107.37(12) . . ? C33 O3 Cu2 127.5(2) . . ? C33 O4 Cu1 129.2(2) . . ? C7 N1 C8 119.1(3) . . ? C7 N1 Cu1 124.1(3) . . ? C8 N1 Cu1 116.6(2) . . ? C19 N2 C12 110.6(3) . . ? C19 N2 C11 110.6(3) . . ? C12 N2 C11 110.1(3) . . ? C19 N2 Cu2 100.4(2) . . ? C12 N2 Cu2 120.9(3) . . ? C11 N2 Cu2 103.5(2) . . ? C21 N3 C20 110.1(3) . . ? C21 N3 C27 111.4(3) . . ? C20 N3 C27 110.5(3) . . ? C21 N3 Cu2 109.4(2) . . ? C20 N3 Cu2 109.2(2) . . ? C27 N3 Cu2 106.2(2) . . ? C22 N4 C26 118.6(3) . . ? C22 N4 Cu2 116.1(2) . . ? C26 N4 Cu2 125.1(3) . . ? C28 N5 C32 118.1(3) . . ? C28 N5 Cu1 127.0(3) . . ? C32 N5 Cu1 113.2(2) . . ? O1 C1 C2 118.9(4) . . ? O1 C1 C6 123.8(4) . . ? C2 C1 C6 117.3(3) . . ? C3 C2 C1 122.2(4) . . ? C2 C3 C4 120.7(4) . . ? C5 C4 C3 118.5(4) . . ? C4 C5 C6 122.1(4) . . ? C5 C6 C1 119.1(4) . . ? C5 C6 C7 117.5(4) . . ? C1 C6 C7 123.4(3) . . ? N1 C7 C6 126.6(4) . . ? N1 C8 C9 110.3(3) . . ? C8 C9 C10 114.4(3) . . ? O2 C10 C11 106.3(3) . . ? O2 C10 C9 109.9(3) . . ? C11 C10 C9 112.0(3) . . ? N2 C11 C10 110.3(3) . . ? N2 C12 C13 115.4(3) . . ? C18 C13 C14 118.6(4) . . ? C18 C13 C12 120.7(4) . . ? C14 C13 C12 120.6(4) . . ? C15 C14 C13 119.9(5) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C17 119.6(4) . . ? C16 C17 C18 120.2(5) . . ? C13 C18 C17 121.1(4) . . ? N2 C19 C20 111.4(3) . . ? N3 C20 C19 111.2(3) . . ? N3 C21 C22 112.2(3) . . ? N4 C22 C23 122.0(4) . . ? N4 C22 C21 116.5(3) . . ? C23 C22 C21 121.5(3) . . ? C22 C23 C24 119.2(4) . . ? C25 C24 C23 118.6(4) . . ? C26 C25 C24 119.5(4) . . ? N4 C26 C25 122.1(4) . . ? C28 C27 N3 109.8(3) . . ? N5 C28 C29 122.0(4) . . ? N5 C28 C27 116.4(3) . . ? C29 C28 C27 121.4(3) . . ? C30 C29 C28 118.8(4) . . ? C31 C30 C29 119.3(4) . . ? C30 C31 C32 118.9(4) . . ? N5 C32 C31 122.7(4) . . ? O4 C33 O3 125.9(3) . . ? O4 C33 C34 118.3(3) . . ? O3 C33 C34 115.9(3) . . ? F1 P1 F3 178.2(4) . . ? F1 P1 F2 90.6(3) . . ? F3 P1 F2 90.8(3) . . ? F1 P1 F4 89.9(3) . . ? F3 P1 F4 88.7(3) . . ? F2 P1 F4 179.4(3) . . ? F1 P1 F5 91.6(3) . . ? F3 P1 F5 89.5(3) . . ? F2 P1 F5 91.4(2) . . ? F4 P1 F5 88.9(2) . . ? F1 P1 F6 90.6(3) . . ? F3 P1 F6 88.3(2) . . ? F2 P1 F6 88.00(18) . . ? F4 P1 F6 91.67(19) . . ? F5 P1 F6 177.7(2) . . ? C1' O1' Cu3 129.2(3) . . ? C10' O2' Cu3 122.8(2) . . ? C10' O2' Cu4 110.7(2) . . ? Cu3 O2' Cu4 105.85(11) . . ? C33' O3' Cu4 127.0(2) . . ? C33' O4' Cu3 126.7(2) . . ? C7' N1' C8' 116.6(3) . . ? C7' N1' Cu3 123.1(3) . . ? C8' N1' Cu3 120.2(2) . . ? C19' N2' C12' 111.8(3) . . ? C19' N2' C11' 110.5(3) . . ? C12' N2' C11' 108.4(3) . . ? C19' N2' Cu4 101.7(2) . . ? C12' N2' Cu4 120.7(2) . . ? C11' N2' Cu4 103.2(2) . . ? C21' N3' C20' 110.3(3) . . ? C21' N3' C27' 111.3(3) . . ? C20' N3' C27' 109.5(3) . . ? C21' N3' Cu4 109.7(2) . . ? C20' N3' Cu4 109.4(2) . . ? C27' N3' Cu4 106.5(2) . . ? C22' N4' C26' 118.7(3) . . ? C22' N4' Cu4 115.6(3) . . ? C26' N4' Cu4 125.7(3) . . ? C28' N5' C32' 117.8(3) . . ? C28' N5' Cu3 128.3(3) . . ? C32' N5' Cu3 111.9(2) . . ? O1' C1' C2' 119.3(3) . . ? O1' C1' C6' 123.3(3) . . ? C2' C1' C6' 117.4(3) . . ? C3' C2' C1' 121.5(4) . . ? C2' C3' C4' 120.9(4) . . ? C5' C4' C3' 118.8(4) . . ? C4' C5' C6' 122.0(4) . . ? C5' C6' C1' 119.5(4) . . ? C5' C6' C7' 118.1(3) . . ? C1' C6' C7' 122.4(3) . . ? N1' C7' C6' 127.6(3) . . ? N1' C8' C9' 113.4(3) . . ? C10' C9' C8' 112.8(3) . . ? O2' C10' C11' 108.9(3) . . ? O2' C10' C9' 111.2(3) . . ? C11' C10' C9' 111.0(3) . . ? N2' C11' C10' 111.2(3) . . ? N2' C12' C13' 116.2(3) . . ? C18' C13' C14' 118.6(4) . . ? C18' C13' C12' 121.5(4) . . ? C14' C13' C12' 119.9(4) . . ? C15' C14' C13' 120.5(5) . . ? C16' C15' C14' 120.4(4) . . ? C15' C16' C17' 120.1(4) . . ? C16' C17' C18' 119.8(5) . . ? C13' C18' C17' 120.6(4) . . ? N2' C19' C20' 110.7(3) . . ? N3' C20' C19' 110.6(3) . . ? N3' C21' C22' 112.5(3) . . ? N4' C22' C23' 122.1(4) . . ? N4' C22' C21' 116.4(3) . . ? C23' C22' C21' 121.4(4) . . ? C24' C23' C22' 118.6(4) . . ? C23' C24' C25' 119.0(4) . . ? C26' C25' C24' 119.2(4) . . ? N4' C26' C25' 122.4(4) . . ? C28' C27' N3' 108.9(3) . . ? N5' C28' C29' 121.5(4) . . ? N5' C28' C27' 117.2(3) . . ? C29' C28' C27' 121.0(4) . . ? C30' C29' C28' 119.3(4) . . ? C31' C30' C29' 119.4(4) . . ? C30' C31' C32' 118.6(4) . . ? N5' C32' C31' 123.2(4) . . ? O4' C33' O3' 125.1(3) . . ? O4' C33' C34' 119.2(3) . . ? O3' C33' C34' 115.7(3) . . ? F1' P1' F6' 93.6(3) . . ? F1' P1' F5' 90.3(3) . . ? F6' P1' F5' 176.0(3) . . ? F1' P1' F3' 88.9(2) . . ? F6' P1' F3' 88.9(2) . . ? F5' P1' F3' 90.7(2) . . ? F1' P1' F2' 90.6(3) . . ? F6' P1' F2' 90.6(2) . . ? F5' P1' F2' 89.8(2) . . ? F3' P1' F2' 179.3(2) . . ? F1' P1' F4' 174.5(3) . . ? F6' P1' F4' 91.0(3) . . ? F5' P1' F4' 85.1(2) . . ? F3' P1' F4' 88.1(2) . . ? F2' P1' F4' 92.4(3) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.055 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.078 #===END data_complex_7 _database_code_CSD 170794 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H75 Cu4 F18 N10 O7 P3' _chemical_formula_weight 1809.43 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' 'Cu' 'Cu' 0.3201 1.2651 '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 11.7811(2) _cell_length_b 16.6703(3) _cell_length_c 19.1074(2) _cell_angle_alpha 96.1665(2) _cell_angle_beta 96.5247(6) _cell_angle_gamma 96.2454(5)) _cell_volume 3678.78(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7353 _exptl_absorpt_correction_T_max 0.9743 _exptl_absorpt_process_details 'SADABS, Sheldrick, 98' _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 '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 14528 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.55 _reflns_number_total 6317 _reflns_number_gt 4718 _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^)+(0.1000P)^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 6317 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.1070 _refine_ls_wR_factor_ref 0.2988 _refine_ls_wR_factor_gt 0.2743 _refine_ls_goodness_of_fit_ref 2.024 _refine_ls_restrained_S_all 2.024 _refine_ls_shift/su_max 0.112 _refine_ls_shift/su_mean 0.005 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 Cu1 Cu 1.33142(17) 0.45704(12) 1.26292(8) 0.0281(8) Uani 1 1 d . . . Cu2 Cu 1.31502(17) 0.27147(12) 1.15730(8) 0.0267(8) Uani 1 1 d . . . Cu3 Cu 1.34207(18) 0.10401(13) 1.20204(9) 0.0311(8) Uani 1 1 d . . . Cu4 Cu 1.17340(18) -0.03404(12) 1.27552(9) 0.0324(8) Uani 1 1 d . . . O1 O 1.2334(8) 0.1660(6) 1.1145(4) 0.026(3) Uani 1 1 d . . . O2 O 1.3911(9) 0.3832(6) 1.1957(4) 0.026(3) Uani 1 1 d . . . O3 O 1.2223(9) 0.2694(6) 1.2350(4) 0.026(3) Uani 1 1 d . . . O4 O 1.2542(8) 0.1499(6) 1.2718(5) 0.026(3) Uani 1 1 d . . . O5 O 1.4563(10) 0.1973(6) 1.2235(5) 0.028(3) Uani 1 1 d . . . O6 O 1.2534(9) -0.0054(7) 1.1972(5) 0.035(2) Uiso 1 1 d . . . N1 N 1.3857(11) 0.2864(8) 1.0748(5) 0.026(3) Uiso 1 1 d . . . N2 N 1.4875(10) 0.5389(8) 1.2828(5) 0.024(3) Uiso 1 1 d . . . N3 N 1.2752(12) 0.5370(8) 1.3345(6) 0.037(3) Uiso 1 1 d . . . N4 N 1.3460(10) 0.3940(8) 1.3550(5) 0.026(3) Uiso 1 1 d . . . N5 N 1.1706(11) 0.4647(8) 1.2099(6) 0.029(3) Uiso 1 1 d . . . N6 N 1.4325(13) 0.0509(9) 1.1391(6) 0.037(3) Uiso 1 1 d . . . N7 N 1.1011(12) -0.1523(9) 1.2256(6) 0.039(3) Uiso 1 1 d . . . N8 N 1.0820(13) -0.0621(10) 1.3590(6) 0.047(4) Uiso 1 1 d . . . N9 N 1.0353(11) 0.0361(8) 1.2604(5) 0.031(3) Uiso 1 1 d . . . N10 N 1.3080(13) -0.0019(8) 1.3557(6) 0.036(3) Uiso 1 1 d . . . C1 C 1.2335(14) 0.1326(11) 1.0479(7) 0.029(3) Uiso 1 1 d . . . C2 C 1.1598(16) 0.0605(12) 1.0258(8) 0.046(4) Uiso 1 1 d . . . H2A H 1.1106 0.0388 1.0571 0.055 Uiso 1 1 calc R . . C3 C 1.1589(15) 0.0204(12) 0.9577(8) 0.046(4) Uiso 1 1 d . . . H3A H 1.1084 -0.0283 0.9427 0.055 Uiso 1 1 calc R . . C4 C 1.2312(16) 0.0510(12) 0.9114(8) 0.044(4) Uiso 1 1 d . . . H4A H 1.2313 0.0223 0.8657 0.053 Uiso 1 1 calc R . . C5 C 1.3017(16) 0.1220(12) 0.9315(8) 0.045(4) Uiso 1 1 d . . . H5A H 1.3503 0.1426 0.8996 0.053 Uiso 1 1 calc R . . C6 C 1.3032(15) 0.1653(11) 0.9997(7) 0.035(4) Uiso 1 1 d . . . C7 C 1.3766(14) 0.2407(10) 1.0156(7) 0.031(3) Uiso 1 1 d . . . H7A H 1.4212 0.2578 0.9803 0.037 Uiso 1 1 calc R . . C8 C 1.4705(13) 0.3613(10) 1.0840(6) 0.025(3) Uiso 1 1 d . . . H8A H 1.4713 0.3845 1.0385 0.030 Uiso 1 1 calc R . . H8B H 1.5487 0.3478 1.0990 0.030 Uiso 1 1 calc R . . C9 C 1.4362(14) 0.4221(10) 1.1395(6) 0.030(3) Uiso 1 1 d . . . H9A H 1.3752 0.4514 1.1165 0.036 Uiso 1 1 calc R . . C10 C 1.5418(14) 0.4836(11) 1.1673(7) 0.039(4) Uiso 1 1 d . . . H10A H 1.5988 0.4546 1.1934 0.046 Uiso 1 1 calc R . . H10B H 1.5761 0.5012 1.1256 0.046 Uiso 1 1 calc R . . C11 C 1.5274(15) 0.5587(10) 1.2146(7) 0.036(4) Uiso 1 1 d . . . H11A H 1.6018 0.5942 1.2248 0.044 Uiso 1 1 calc R . . H11B H 1.4707 0.5890 1.1897 0.044 Uiso 1 1 calc R . . C12 C 1.7458(9) 0.6110(6) 1.3446(5) 0.041(4) Uiso 1 1 d G . . H12A H 1.6991 0.6494 1.3273 0.049 Uiso 1 1 calc R . . C13 C 1.8604(10) 0.6355(6) 1.3716(5) 0.054(5) Uiso 1 1 d G . . H13A H 1.8920 0.6906 1.3728 0.065 Uiso 1 1 calc R . . C14 C 1.9288(7) 0.5792(7) 1.3968(5) 0.063(5) Uiso 1 1 d G . . H14A H 2.0071 0.5959 1.4153 0.076 Uiso 1 1 calc R . . C15 C 1.8825(9) 0.4986(7) 1.3951(5) 0.060(5) Uiso 1 1 d G . . H15A H 1.9292 0.4602 1.4123 0.071 Uiso 1 1 calc R . . C16 C 1.7679(9) 0.4742(5) 1.3681(5) 0.045(4) Uiso 1 1 d G . . H16A H 1.7363 0.4191 1.3668 0.053 Uiso 1 1 calc R . . C17 C 1.6996(7) 0.5304(7) 1.3428(5) 0.035(4) Uiso 1 1 d G . . C18 C 1.5704(13) 0.4979(10) 1.3255(7) 0.034(4) Uiso 1 1 d . . . H18A H 1.5661 0.4418 1.3015 0.041 Uiso 1 1 calc R . . H18B H 1.5407 0.4934 1.3715 0.041 Uiso 1 1 calc R . . C19 C 1.4591(15) 0.6149(11) 1.3244(7) 0.038(4) Uiso 1 1 d . . . H19A H 1.4248 0.6501 1.2913 0.046 Uiso 1 1 calc R . . H19B H 1.5306 0.6456 1.3508 0.046 Uiso 1 1 calc R . . C20 C 1.3750(16) 0.5934(12) 1.3762(8) 0.050(4) Uiso 1 1 d . . . H20A H 1.4128 0.5662 1.4145 0.060 Uiso 1 1 calc R . . H20B H 1.3476 0.6432 1.3980 0.060 Uiso 1 1 calc R . . C21 C 1.2177(15) 0.4886(10) 1.3862(8) 0.040(4) Uiso 1 1 d . . . H21A H 1.2099 0.5250 1.4294 0.049 Uiso 1 1 calc R . . H21B H 1.1398 0.4641 1.3643 0.049 Uiso 1 1 calc R . . C22 C 1.2891(14) 0.4228(10) 1.4056(7) 0.030(3) Uiso 1 1 d . . . C23 C 1.2929(15) 0.3948(11) 1.4698(8) 0.046(4) Uiso 1 1 d . . . H23A H 1.2496 0.4169 1.5046 0.055 Uiso 1 1 calc R . . C24 C 1.3588(15) 0.3349(11) 1.4843(8) 0.040(4) Uiso 1 1 d . . . H24A H 1.3634 0.3156 1.5294 0.049 Uiso 1 1 calc R . . C25 C 1.4191(15) 0.3024(11) 1.4319(7) 0.042(4) Uiso 1 1 d . . . H25A H 1.4668 0.2611 1.4405 0.050 Uiso 1 1 calc R . . C26 C 1.4076(14) 0.3320(10) 1.3662(7) 0.036(4) Uiso 1 1 d . . . H26A H 1.4439 0.3081 1.3286 0.043 Uiso 1 1 calc R . . C27 C 1.1890(14) 0.5831(10) 1.2964(7) 0.038(4) Uiso 1 1 d . . . H27A H 1.1380 0.6048 1.3297 0.046 Uiso 1 1 calc R . . H27B H 1.2292 0.6293 1.2769 0.046 Uiso 1 1 calc R . . C28 C 1.1195(14) 0.5249(11) 1.2374(7) 0.032(3) Uiso 1 1 d . . . C29 C 1.0051(14) 0.5395(11) 1.2125(7) 0.041(4) Uiso 1 1 d . . . H29A H 0.9685 0.5825 1.2333 0.049 Uiso 1 1 calc R . . C30 C 0.9514(15) 0.4830(11) 1.1533(7) 0.039(4) Uiso 1 1 d . . . H30A H 0.8752 0.4887 1.1341 0.047 Uiso 1 1 calc R . . C31 C 1.0026(14) 0.4223(11) 1.1232(7) 0.036(4) Uiso 1 1 d . . . H31A H 0.9639 0.3859 1.0840 0.044 Uiso 1 1 calc R . . C32 C 1.1192(15) 0.4143(11) 1.1530(7) 0.042(4) Uiso 1 1 d . . . H32A H 1.1592 0.3733 1.1321 0.050 Uiso 1 1 calc R . . C33 C 1.2106(15) 0.2149(11) 1.2754(7) 0.032(4) Uiso 1 1 d . . . C34 C 1.1367(15) 0.2312(11) 1.3333(7) 0.045(4) Uiso 1 1 d . . . H34A H 1.1089 0.2842 1.3304 0.067 Uiso 1 1 calc R . . H34B H 1.1822 0.2314 1.3796 0.067 Uiso 1 1 calc R . . H34C H 1.0709 0.1886 1.3276 0.067 Uiso 1 1 calc R . . C35 C 1.5534(17) 0.2108(11) 1.1965(7) 0.029(3) Uiso 1 1 d . . . C36 C 1.6322(16) 0.2767(12) 1.2234(8) 0.046(4) Uiso 1 1 d . . . H36A H 1.6205 0.3077 1.2661 0.055 Uiso 1 1 calc R . . C37 C 1.7305(17) 0.3008(12) 1.1904(8) 0.050(4) Uiso 1 1 d . . . H37A H 1.7820 0.3477 1.2099 0.060 Uiso 1 1 calc R . . C38 C 1.7502(17) 0.2536(12) 1.1281(8) 0.049(4) Uiso 1 1 d . . . H38A H 1.8129 0.2702 1.1036 0.059 Uiso 1 1 calc R . . C39 C 1.6784(16) 0.1839(12) 1.1032(8) 0.047(4) Uiso 1 1 d . . . H39A H 1.6930 0.1509 1.0623 0.057 Uiso 1 1 calc R . . C40 C 1.5822(15) 0.1606(11) 1.1382(7) 0.033(4) Uiso 1 1 d . . . C41 C 1.5222(16) 0.0808(12) 1.1125(8) 0.042(4) Uiso 1 1 d . . . H41A H 1.5493 0.0491 1.0750 0.051 Uiso 1 1 calc R . . C42 C 1.3802(17) -0.0340(12) 1.1122(8) 0.055(5) Uiso 1 1 d . . . H42A H 1.3250 -0.0339 1.0691 0.066 Uiso 1 1 calc R . . H42B H 1.4410 -0.0675 1.0996 0.066 Uiso 1 1 calc R . . C43 C 1.3203(15) -0.0685(11) 1.1675(8) 0.041(4) Uiso 1 1 d . . . H43A H 1.3796 -0.0791 1.2061 0.049 Uiso 1 1 calc R . . C44 C 1.2457(16) -0.1487(12) 1.1395(8) 0.050(5) Uiso 1 1 d . . . H44A H 1.1844 -0.1375 1.1032 0.060 Uiso 1 1 calc R . . H44B H 1.2940 -0.1850 1.1152 0.060 Uiso 1 1 calc R . . C45 C 1.1909(15) -0.1930(11) 1.1916(8) 0.041(4) Uiso 1 1 d . . . H45A H 1.2514 -0.2019 1.2294 0.049 Uiso 1 1 calc R . . H45B H 1.1555 -0.2471 1.1679 0.049 Uiso 1 1 calc R . . C46 C 0.9581(9) -0.2689(9) 1.0797(6) 0.061(5) Uiso 1 1 d G . . H46A H 1.0263 -0.2504 1.0611 0.073 Uiso 1 1 calc R . . C47 C 0.8900(12) -0.3395(8) 1.0476(5) 0.062(5) Uiso 1 1 d G . . H47A H 0.9117 -0.3692 1.0070 0.075 Uiso 1 1 calc R . . C48 C 0.7902(11) -0.3666(7) 1.0748(6) 0.055(5) Uiso 1 1 d G . . H48A H 0.7436 -0.4148 1.0528 0.066 Uiso 1 1 calc R . . C49 C 0.7584(9) -0.3232(9) 1.1342(6) 0.069(6) Uiso 1 1 d G . . H49A H 0.6901 -0.3417 1.1528 0.083 Uiso 1 1 calc R . . C50 C 0.8264(12) -0.2526(8) 1.1664(5) 0.073(6) Uiso 1 1 d G . . H50A H 0.8047 -0.2229 1.2069 0.087 Uiso 1 1 calc R . . C51 C 0.9263(12) -0.2255(6) 1.1391(6) 0.045(4) Uiso 1 1 d G . . C52 C 0.9988(15) -0.1462(11) 1.1737(7) 0.042(4) Uiso 1 1 d . . . H52A H 1.0258 -0.1165 1.1354 0.050 Uiso 1 1 calc R . . H52B H 0.9477 -0.1124 1.1982 0.050 Uiso 1 1 calc R . . C53 C 1.0694(17) -0.1959(13) 1.2865(9) 0.059(5) Uiso 1 1 d . . . H53A H 1.0162 -0.2458 1.2685 0.071 Uiso 1 1 calc R . . H53B H 1.1394 -0.2120 1.3124 0.071 Uiso 1 1 calc R . . C54 C 1.0144(17) -0.1429(13) 1.3344(9) 0.056(5) Uiso 1 1 d . . . H54A H 1.0004 -0.1707 1.3764 0.067 Uiso 1 1 calc R . . H54B H 0.9386 -0.1345 1.3100 0.067 Uiso 1 1 calc R . . C55 C 1.0143(16) 0.0037(11) 1.3759(8) 0.046(4) Uiso 1 1 d . . . H55A H 1.0623 0.0463 1.4102 0.055 Uiso 1 1 calc R . . H55B H 0.9479 -0.0173 1.3989 0.055 Uiso 1 1 calc R . . C56 C 0.9714(15) 0.0406(11) 1.3117(8) 0.041(4) Uiso 1 1 d . . . C57 C 0.8709(18) 0.0794(12) 1.3066(9) 0.065(5) Uiso 1 1 d . . . H57A H 0.8205 0.0775 1.3419 0.078 Uiso 1 1 calc R . . C58 C 0.8488(16) 0.1195(11) 1.2495(8) 0.051(5) Uiso 1 1 d . . . H58A H 0.7826 0.1473 1.2448 0.061 Uiso 1 1 calc R . . C59 C 0.9211(15) 0.1201(11) 1.1987(7) 0.041(4) Uiso 1 1 d . . . H59A H 0.9073 0.1500 1.1597 0.049 Uiso 1 1 calc R . . C60 C 1.0140(13) 0.0774(9) 1.2044(7) 0.030(3) Uiso 1 1 d . . . H60A H 1.0638 0.0768 1.1686 0.036 Uiso 1 1 calc R . . C61 C 1.1718(15) -0.0696(11) 1.4197(8) 0.045(4) Uiso 1 1 d . . . H61A H 1.1390 -0.0612 1.4650 0.053 Uiso 1 1 calc R . . H61B H 1.1954 -0.1249 1.4148 0.053 Uiso 1 1 calc R . . C62 C 1.2744(15) -0.0082(11) 1.4208(7) 0.039(4) Uiso 1 1 d . . . C63 C 1.3392(16) 0.0318(11) 1.4830(8) 0.047(4) Uiso 1 1 d . . . H63A H 1.3156 0.0257 1.5283 0.056 Uiso 1 1 calc R . . C64 C 1.4376(17) 0.0799(12) 1.4762(8) 0.050(5) Uiso 1 1 d . . . H64A H 1.4811 0.1107 1.5170 0.060 Uiso 1 1 calc R . . C65 C 1.4734(18) 0.0841(12) 1.4130(9) 0.061(5) Uiso 1 1 d . . . H65A H 1.5437 0.1162 1.4093 0.073 Uiso 1 1 calc R . . C66 C 1.4077(16) 0.0415(11) 1.3518(7) 0.039(4) Uiso 1 1 d . . . H66A H 1.4351 0.0437 1.3071 0.047 Uiso 1 1 calc R . . P1 P 0.2847(4) 0.6155(3) 0.0436(2) 0.0344(18) Uani 1 1 d . . . F1 F 0.2122(11) 0.5340(7) 0.0511(6) 0.071(4) Uani 1 1 d . . . F2 F 0.1716(9) 0.6596(7) 0.0338(5) 0.067(4) Uani 1 1 d . . . F3 F 0.3603(9) 0.6995(6) 0.0380(4) 0.051(3) Uani 1 1 d . . . F4 F 0.4015(9) 0.5734(6) 0.0533(4) 0.060(4) Uani 1 1 d . . . F5 F 0.2756(8) 0.5924(6) -0.0405(4) 0.043(3) Uani 1 1 d . . . F6 F 0.2916(9) 0.6405(7) 0.1281(4) 0.060(4) Uani 1 1 d . . . P2 P 0.7950(5) 0.2611(4) 0.4725(2) 0.044(2) Uani 1 1 d . . . F7 F 0.6872(15) 0.2263(11) 0.5054(9) 0.140(7) Uani 1 1 d . . . F8 F 0.8087(19) 0.1710(9) 0.4553(6) 0.164(9) Uani 1 1 d . . . F9 F 0.8970(17) 0.2958(13) 0.4424(10) 0.178(9) Uani 1 1 d . . . F10 F 0.7749(19) 0.3506(8) 0.4909(7) 0.162(9) Uani 1 1 d . . . F11 F 0.8568(13) 0.2642(7) 0.5497(6) 0.117(6) Uani 1 1 d . . . F12 F 0.7270(19) 0.2577(9) 0.3981(6) 0.181(9) Uani 1 1 d . . . P3 P 0.3821(8) -0.8497(5) 0.6923(3) 0.079(3) Uani 1 1 d . . . F13 F 0.3953(17) -0.9334(13) 0.6550(9) 0.145(6) Uiso 1 1 d . . . F14 F 0.380(2) -0.8073(9) 0.6215(7) 0.174(9) Uani 1 1 d . . . F15 F 0.3827(19) -0.7687(11) 0.7317(8) 0.164(9) Uani 1 1 d . . . F16 F 0.374(3) -0.8846(10) 0.7580(9) 0.33(2) Uani 1 1 d . . . F17 F 0.259(4) -0.874(2) 0.671(2) 0.336(18) Uiso 1 1 d . . . F18 F 0.5141(18) -0.833(2) 0.6905(15) 0.298(19) Uani 1 1 d . . . O7 O 1.112(3) 0.153(2) 1.5128(18) 0.290(16) 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 Cu1 0.0282(16) 0.0252(17) 0.0295(9) -0.0003(10) 0.0002(9) 0.0040(13) Cu2 0.0309(16) 0.0225(19) 0.0262(8) -0.0003(10) 0.0030(9) 0.0043(14) Cu3 0.0332(17) 0.0256(19) 0.0335(9) -0.0005(10) 0.0046(10) 0.0024(15) Cu4 0.0456(17) 0.0170(17) 0.0348(9) 0.0023(10) 0.0031(10) 0.0078(13) O1 0.024(8) 0.024(9) 0.025(4) -0.002(5) 0.000(5) -0.012(7) O2 0.028(8) 0.018(9) 0.029(4) 0.010(5) 0.001(5) -0.019(7) O3 0.026(8) 0.029(8) 0.028(4) 0.006(5) 0.015(5) 0.007(7) O4 0.012(7) 0.024(9) 0.044(5) 0.004(6) 0.007(5) 0.003(7) O5 0.020(9) 0.017(9) 0.048(5) 0.008(6) 0.009(6) -0.004(8) P1 0.039(4) 0.030(5) 0.037(2) -0.002(3) 0.011(2) 0.016(4) F1 0.077(11) 0.046(10) 0.099(8) 0.008(7) 0.064(8) -0.006(9) F2 0.054(8) 0.075(10) 0.074(6) 0.003(6) 0.005(6) 0.033(8) F3 0.070(9) 0.012(8) 0.060(5) -0.011(5) -0.010(5) -0.006(7) F4 0.077(9) 0.067(9) 0.052(5) 0.023(6) 0.020(5) 0.055(7) F5 0.051(8) 0.033(8) 0.040(4) -0.015(5) 0.001(5) 0.008(6) F6 0.071(9) 0.078(10) 0.038(5) -0.001(5) 0.021(5) 0.030(8) P2 0.057(5) 0.038(5) 0.038(2) 0.007(3) 0.006(3) 0.013(4) F7 0.107(15) 0.150(18) 0.166(14) 0.042(13) 0.038(12) -0.013(13) F8 0.37(3) 0.083(13) 0.078(9) 0.020(9) 0.072(13) 0.136(16) F9 0.16(2) 0.19(2) 0.217(19) 0.083(16) 0.140(18) -0.001(17) F10 0.37(3) 0.058(12) 0.095(10) 0.031(9) 0.077(13) 0.107(15) F11 0.174(14) 0.064(10) 0.084(7) 0.022(7) -0.069(8) -0.042(10) F12 0.33(3) 0.104(13) 0.077(8) 0.034(9) -0.094(12) -0.016(15) P3 0.133(9) 0.036(6) 0.064(3) -0.023(4) -0.013(4) 0.040(5) F14 0.35(3) 0.078(13) 0.088(9) 0.005(9) -0.028(13) 0.070(15) F15 0.29(3) 0.076(15) 0.107(10) -0.009(10) 0.080(13) -0.094(16) F16 0.86(7) 0.081(15) 0.105(12) 0.015(10) 0.24(3) 0.08(2) F18 0.074(17) 0.54(5) 0.36(3) 0.25(4) 0.10(2) 0.12(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 Cu1 O2 1.927(11) . ? Cu1 N3 2.023(14) . ? Cu1 N5 2.068(11) . ? Cu1 N2 2.138(13) . ? Cu1 N4 2.144(9) . ? Cu2 N1 1.891(11) . ? Cu2 O3 1.941(9) . ? Cu2 O1 1.957(11) . ? Cu2 O2 2.001(11) . ? Cu2 Cu3 3.045(3) . ? Cu3 N6 1.906(15) . ? Cu3 O5 1.918(12) . ? Cu3 O4 1.923(11) . ? Cu3 O6 1.988(12) . ? Cu3 O1 2.382(8) . ? Cu4 O6 1.932(10) . ? Cu4 N10 2.058(13) . ? Cu4 N8 2.089(14) . ? Cu4 N9 2.116(12) . ? Cu4 N7 2.138(15) . ? O1 C1 1.333(17) . ? O2 C9 1.435(16) . ? O3 C33 1.260(16) . ? O4 C33 1.247(18) . ? O5 C35 1.315(19) . ? O6 C43 1.484(19) . ? N1 C7 1.282(18) . ? N1 C8 1.493(18) . ? N2 C18 1.473(16) . ? N2 C11 1.492(17) . ? N2 C19 1.513(19) . ? N3 C27 1.508(17) . ? N3 C20 1.51(2) . ? N3 C21 1.514(19) . ? N4 C22 1.317(18) . ? N4 C26 1.347(19) . ? N5 C28 1.317(18) . ? N5 C32 1.34(2) . ? N6 C41 1.297(19) . ? N6 C42 1.49(2) . ? N7 C45 1.49(2) . ? N7 C52 1.490(18) . ? N7 C53 1.498(19) . ? N8 C55 1.46(2) . ? N8 C54 1.49(2) . ? N8 C61 1.504(17) . ? N9 C56 1.303(19) . ? N9 C60 1.347(15) . ? N10 C66 1.324(18) . ? N10 C62 1.360(19) . ? C1 C2 1.40(2) . ? C1 C6 1.41(2) . ? C2 C3 1.40(2) . ? C3 C4 1.39(2) . ? C4 C5 1.36(2) . ? C5 C6 1.42(2) . ? C6 C7 1.43(2) . ? C8 C9 1.51(2) . ? C9 C10 1.53(2) . ? C10 C11 1.50(2) . ? C12 C13 1.3900 . ? C12 C17 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.545(17) . ? C19 C20 1.52(2) . ? C21 C22 1.51(2) . ? C22 C23 1.356(18) . ? C23 C24 1.36(2) . ? C24 C25 1.39(2) . ? C25 C26 1.397(17) . ? C27 C28 1.51(2) . ? C28 C29 1.43(2) . ? C29 C30 1.43(2) . ? C30 C31 1.34(2) . ? C31 C32 1.45(2) . ? C33 C34 1.50(2) . ? C35 C36 1.37(2) . ? C35 C40 1.41(2) . ? C36 C37 1.42(2) . ? C37 C38 1.41(2) . ? C38 C39 1.37(2) . ? C39 C40 1.42(2) . ? C40 C41 1.45(2) . ? C42 C43 1.47(2) . ? C43 C44 1.53(2) . ? C44 C45 1.47(2) . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.534(19) . ? C53 C54 1.46(2) . ? C55 C56 1.492(17) . ? C56 C57 1.41(2) . ? C57 C58 1.35(2) . ? C58 C59 1.36(2) . ? C59 C60 1.37(2) . ? C61 C62 1.49(2) . ? C62 C63 1.40(2) . ? C63 C64 1.36(2) . ? C64 C65 1.33(2) . ? C65 C66 1.40(2) . ? P1 F1 1.555(12) . ? P1 F2 1.592(10) . ? P1 F3 1.596(11) . ? P1 F5 1.600(9) . ? P1 F4 1.612(10) . ? P1 F6 1.615(9) . ? P2 F9 1.479(16) . ? P2 F8 1.532(14) . ? P2 F12 1.542(11) . ? P2 F10 1.547(14) . ? P2 F11 1.562(10) . ? P2 F7 1.563(16) . ? P3 F16 1.450(14) . ? P3 F17 1.46(4) . ? P3 F15 1.472(18) . ? P3 F13 1.53(2) . ? P3 F18 1.56(2) . ? P3 F14 1.589(14) . ? 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 O2 Cu1 N3 177.7(5) . . ? O2 Cu1 N5 101.1(5) . . ? N3 Cu1 N5 80.8(5) . . ? O2 Cu1 N2 93.6(5) . . ? N3 Cu1 N2 84.2(5) . . ? N5 Cu1 N2 132.8(4) . . ? O2 Cu1 N4 100.7(4) . . ? N3 Cu1 N4 79.4(5) . . ? N5 Cu1 N4 119.8(5) . . ? N2 Cu1 N4 100.8(4) . . ? N1 Cu2 O3 169.2(4) . . ? N1 Cu2 O1 92.1(5) . . ? O3 Cu2 O1 89.6(4) . . ? N1 Cu2 O2 86.3(5) . . ? O3 Cu2 O2 91.2(4) . . ? O1 Cu2 O2 175.7(3) . . ? N1 Cu2 Cu3 110.9(4) . . ? O3 Cu2 Cu3 78.4(3) . . ? O1 Cu2 Cu3 51.4(2) . . ? O2 Cu2 Cu3 132.9(2) . . ? N6 Cu3 O5 91.7(6) . . ? N6 Cu3 O4 174.4(4) . . ? O5 Cu3 O4 90.1(5) . . ? N6 Cu3 O6 84.7(6) . . ? O5 Cu3 O6 164.6(4) . . ? O4 Cu3 O6 92.1(5) . . ? N6 Cu3 O1 96.4(4) . . ? O5 Cu3 O1 92.3(3) . . ? O4 Cu3 O1 88.8(3) . . ? O6 Cu3 O1 102.9(4) . . ? N6 Cu3 Cu2 108.0(4) . . ? O5 Cu3 Cu2 54.7(3) . . ? O4 Cu3 Cu2 77.3(3) . . ? O6 Cu3 Cu2 140.5(3) . . ? O1 Cu3 Cu2 40.0(3) . . ? O6 Cu4 N10 98.2(5) . . ? O6 Cu4 N8 177.7(5) . . ? N10 Cu4 N8 83.2(5) . . ? O6 Cu4 N9 98.7(4) . . ? N10 Cu4 N9 122.5(5) . . ? N8 Cu4 N9 79.0(5) . . ? O6 Cu4 N7 95.3(5) . . ? N10 Cu4 N7 129.2(5) . . ? N8 Cu4 N7 85.2(6) . . ? N9 Cu4 N7 103.2(5) . . ? C1 O1 Cu2 125.9(10) . . ? C1 O1 Cu3 114.8(9) . . ? Cu2 O1 Cu3 88.6(3) . . ? C9 O2 Cu1 113.1(9) . . ? C9 O2 Cu2 109.4(8) . . ? Cu1 O2 Cu2 124.8(5) . . ? C33 O3 Cu2 127.4(11) . . ? C33 O4 Cu3 129.9(10) . . ? C35 O5 Cu3 128.1(12) . . ? C43 O6 Cu4 115.0(8) . . ? C43 O6 Cu3 109.9(9) . . ? Cu4 O6 Cu3 120.2(6) . . ? C7 N1 C8 116.8(13) . . ? C7 N1 Cu2 130.3(13) . . ? C8 N1 Cu2 112.8(8) . . ? C18 N2 C11 112.9(12) . . ? C18 N2 C19 111.4(10) . . ? C11 N2 C19 109.9(11) . . ? C18 N2 Cu1 105.9(9) . . ? C11 N2 Cu1 110.5(9) . . ? C19 N2 Cu1 106.0(9) . . ? C27 N3 C20 111.9(13) . . ? C27 N3 C21 109.7(13) . . ? C20 N3 C21 107.7(11) . . ? C27 N3 Cu1 109.1(9) . . ? C20 N3 Cu1 110.8(11) . . ? C21 N3 Cu1 107.5(10) . . ? C22 N4 C26 118.9(11) . . ? C22 N4 Cu1 113.6(9) . . ? C26 N4 Cu1 127.5(11) . . ? C28 N5 C32 121.1(14) . . ? C28 N5 Cu1 113.8(10) . . ? C32 N5 Cu1 125.1(12) . . ? C41 N6 C42 118.4(17) . . ? C41 N6 Cu3 129.2(15) . . ? C42 N6 Cu3 112.0(12) . . ? C45 N7 C52 112.1(12) . . ? C45 N7 C53 109.2(12) . . ? C52 N7 C53 112.2(14) . . ? C45 N7 Cu4 109.5(11) . . ? C52 N7 Cu4 110.1(10) . . ? C53 N7 Cu4 103.3(10) . . ? C55 N8 C54 115.4(15) . . ? C55 N8 C61 111.6(13) . . ? C54 N8 C61 109.6(13) . . ? C55 N8 Cu4 108.4(10) . . ? C54 N8 Cu4 105.6(10) . . ? C61 N8 Cu4 105.5(11) . . ? C56 N9 C60 120.0(13) . . ? C56 N9 Cu4 115.2(9) . . ? C60 N9 Cu4 124.8(11) . . ? C66 N10 C62 118.3(14) . . ? C66 N10 Cu4 127.0(9) . . ? C62 N10 Cu4 112.1(12) . . ? O1 C1 C2 116.7(14) . . ? O1 C1 C6 124.1(17) . . ? C2 C1 C6 119.2(15) . . ? C3 C2 C1 119.8(17) . . ? C4 C3 C2 120.8(19) . . ? C5 C4 C3 120.2(17) . . ? C4 C5 C6 120.6(17) . . ? C1 C6 C5 119.3(18) . . ? C1 C6 C7 123.7(15) . . ? C5 C6 C7 117.0(15) . . ? N1 C7 C6 123.6(15) . . ? N1 C8 C9 108.7(13) . . ? O2 C9 C8 111.6(12) . . ? O2 C9 C10 111.7(10) . . ? C8 C9 C10 107.9(14) . . ? C11 C10 C9 119.0(15) . . ? N2 C11 C10 111.8(13) . . ? C13 C12 C17 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C12 120.0 . . ? C16 C17 C18 114.1(9) . . ? C12 C17 C18 125.2(9) . . ? N2 C18 C17 123.1(12) . . ? N2 C19 C20 110.7(14) . . ? N3 C20 C19 107.1(13) . . ? C22 C21 N3 109.4(14) . . ? N4 C22 C23 122.9(14) . . ? N4 C22 C21 114.6(11) . . ? C23 C22 C21 122.6(16) . . ? C22 C23 C24 119.9(18) . . ? C23 C24 C25 118.9(14) . . ? C24 C25 C26 118.1(15) . . ? N4 C26 C25 121.2(16) . . ? C28 C27 N3 107.6(13) . . ? N5 C28 C29 124.0(15) . . ? N5 C28 C27 117.0(14) . . ? C29 C28 C27 119.0(16) . . ? C30 C29 C28 113.4(17) . . ? C31 C30 C29 123.8(16) . . ? C30 C31 C32 117.5(16) . . ? N5 C32 C31 120.1(17) . . ? O4 C33 O3 126.4(16) . . ? O4 C33 C34 117.8(13) . . ? O3 C33 C34 115.8(15) . . ? O5 C35 C36 120.7(18) . . ? O5 C35 C40 123.1(18) . . ? C36 C35 C40 116.2(19) . . ? C35 C36 C37 123.0(19) . . ? C38 C37 C36 119(2) . . ? C39 C38 C37 119.5(19) . . ? C38 C39 C40 120.3(19) . . ? C35 C40 C39 121.5(19) . . ? C35 C40 C41 123.6(18) . . ? C39 C40 C41 114.9(17) . . ? N6 C41 C40 122.1(18) . . ? C43 C42 N6 109.2(15) . . ? C42 C43 O6 107.0(14) . . ? C42 C43 C44 112.2(15) . . ? O6 C43 C44 112.9(15) . . ? C45 C44 C43 117.0(14) . . ? C44 C45 N7 115.4(14) . . ? C47 C46 C51 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 C52 119.6(12) . . ? C46 C51 C52 120.4(12) . . ? N7 C52 C51 117.8(12) . . ? C54 C53 N7 109.7(15) . . ? C53 C54 N8 114.4(17) . . ? N8 C55 C56 112.3(14) . . ? N9 C56 C57 121.6(13) . . ? N9 C56 C55 115.1(15) . . ? C57 C56 C55 123.2(16) . . ? C58 C57 C56 117.7(19) . . ? C57 C58 C59 120.2(18) . . ? C58 C59 C60 119.6(14) . . ? N9 C60 C59 120.5(15) . . ? C62 C61 N8 110.5(12) . . ? N10 C62 C63 122.3(18) . . ? N10 C62 C61 113.5(14) . . ? C63 C62 C61 123.8(15) . . ? C64 C63 C62 117.3(16) . . ? C65 C64 C63 120.9(19) . . ? C64 C65 C66 120(2) . . ? N10 C66 C65 120.8(16) . . ? F1 P1 F2 91.2(7) . . ? F1 P1 F3 178.5(5) . . ? F2 P1 F3 89.3(6) . . ? F1 P1 F5 91.2(6) . . ? F2 P1 F5 90.3(5) . . ? F3 P1 F5 90.3(5) . . ? F1 P1 F4 90.5(7) . . ? F2 P1 F4 178.3(7) . . ? F3 P1 F4 89.1(6) . . ? F5 P1 F4 89.7(5) . . ? F1 P1 F6 89.2(6) . . ? F2 P1 F6 88.3(6) . . ? F3 P1 F6 89.3(6) . . ? F5 P1 F6 178.6(6) . . ? F4 P1 F6 91.7(5) . . ? F9 P2 F8 98.1(11) . . ? F9 P2 F12 87.3(11) . . ? F8 P2 F12 88.6(8) . . ? F9 P2 F10 84.9(11) . . ? F8 P2 F10 177.0(12) . . ? F12 P2 F10 91.0(9) . . ? F9 P2 F11 95.9(10) . . ? F8 P2 F11 92.1(8) . . ? F12 P2 F11 176.5(12) . . ? F10 P2 F11 88.1(8) . . ? F9 P2 F7 178.6(12) . . ? F8 P2 F7 83.2(10) . . ? F12 P2 F7 93.2(11) . . ? F10 P2 F7 93.8(10) . . ? F11 P2 F7 83.5(9) . . ? F16 P3 F17 90(2) . . ? F16 P3 F15 88.7(9) . . ? F17 P3 F15 101.6(19) . . ? F16 P3 F13 89.7(10) . . ? F17 P3 F13 84.6(17) . . ? F15 P3 F13 173.6(13) . . ? F16 P3 F18 103.4(18) . . ? F17 P3 F18 163(2) . . ? F15 P3 F18 90.5(17) . . ? F13 P3 F18 83.9(15) . . ? F16 P3 F14 174.0(17) . . ? F17 P3 F14 86.2(16) . . ? F15 P3 F14 88.0(8) . . ? F13 P3 F14 94.0(8) . . ? F18 P3 F14 81.6(12) . . ? _diffrn_measured_fraction_theta_max 0.412 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.412 _refine_diff_density_max 1.163 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.148 #===END data_complex_8 _database_code_CSD 170795 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H80 Cu4 F24 N14 O6 P4' _chemical_formula_weight 1999.48 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' 'Cu' 'Cu' 0.3201 1.2651 '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 11.5418(6) _cell_length_b 13.7097(7) _cell_length_c 14.0734(8) _cell_angle_alpha 69.5232(11) _cell_angle_beta 83.0061(13) _cell_angle_gamma 77.5450(11) _cell_volume 2034.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4786 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6742 _exptl_absorpt_correction_T_max 0.9414 _exptl_absorpt_process_details 'Sadabs, Sheldrick, 1998' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 12181 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7060 _reflns_number_gt 4908 _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^)+(0.1000P)^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 7060 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.308 _refine_ls_restrained_S_all 1.308 _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 Cu1 Cu 0.79990(7) 0.32191(6) 0.24663(6) 0.0405(3) Uani 1 1 d . . . Cu2 Cu 0.54875(6) 0.58626(6) 0.41531(6) 0.0336(2) Uani 1 1 d . . . P1 P 1.01898(17) -0.14761(16) 0.26454(15) 0.0483(5) Uani 1 1 d . . . P2 P 0.3404(2) 0.2243(2) 0.04714(19) 0.0722(7) Uani 1 1 d . . . N1 N 0.7058(5) 0.6346(4) 0.3973(4) 0.0391(13) Uani 1 1 d . . . N2 N 0.5667(5) 0.8729(4) 0.2118(4) 0.0436(14) Uani 1 1 d . . . N3 N 0.4992(4) 0.7316(4) 0.3141(4) 0.0376(13) Uani 1 1 d . . . N4 N 0.7665(4) 0.2128(4) 0.3989(4) 0.0397(13) Uani 1 1 d . . . N5 N 0.9657(4) 0.2294(4) 0.2578(4) 0.0420(14) Uani 1 1 d . . . N6 N 0.9008(5) 0.4396(4) 0.2119(4) 0.0397(13) Uani 1 1 d . . . N7 N 0.7921(5) 0.2584(5) 0.1338(4) 0.0441(14) Uani 1 1 d . . . O1 O 0.4009(3) 0.5403(3) 0.4728(3) 0.0360(10) Uani 1 1 d . . . O2 O 0.6187(4) 0.5126(4) 0.2953(4) 0.0517(13) Uani 1 1 d . . . O3 O 0.6384(4) 0.3917(4) 0.2221(4) 0.0565(14) Uani 1 1 d . . . C1 C 0.7062(6) 0.7249(5) 0.3304(5) 0.0422(17) Uani 1 1 d . . . H1A H 0.7746 0.7555 0.3122 0.051 Uiso 1 1 calc R . . C2 C 0.5938(5) 0.7778(5) 0.2839(5) 0.0388(16) Uani 1 1 d . . . C3 C 0.4485(6) 0.8876(5) 0.1927(5) 0.0459(17) Uani 1 1 d . . . H3A H 0.4045 0.9465 0.1452 0.055 Uiso 1 1 calc R . . C4 C 0.4083(6) 0.7993(5) 0.2568(5) 0.0438(17) Uani 1 1 d . . . H4A H 0.3306 0.7871 0.2608 0.053 Uiso 1 1 calc R . . C5 C 0.6471(7) 0.9474(5) 0.1579(6) 0.057(2) Uani 1 1 d . . . H5A H 0.7254 0.9194 0.1849 0.085 Uiso 1 1 calc R . . H5B H 0.6163 1.0153 0.1671 0.085 Uiso 1 1 calc R . . H5C H 0.6525 0.9565 0.0860 0.085 Uiso 1 1 calc R . . C6 C 0.8172(5) 0.5718(5) 0.4452(6) 0.0452(18) Uani 1 1 d . . . H6A H 0.8650 0.6193 0.4531 0.054 Uiso 1 1 calc R . . H6B H 0.8633 0.5336 0.4015 0.054 Uiso 1 1 calc R . . C7 C 0.7905(6) 0.4928(5) 0.5490(6) 0.0467(18) Uani 1 1 d . . . H7A H 0.7461 0.5325 0.5920 0.056 Uiso 1 1 calc R . . H7B H 0.8660 0.4554 0.5804 0.056 Uiso 1 1 calc R . . C8 C 0.7199(5) 0.4102(5) 0.5488(5) 0.0357(15) Uani 1 1 d . . . H8A H 0.7203 0.3571 0.6179 0.043 Uiso 1 1 calc R . . C9 C 0.7780(5) 0.3526(5) 0.4753(5) 0.0375(15) Uani 1 1 d . . . H9A H 0.8606 0.3212 0.4930 0.045 Uiso 1 1 calc R . . H9B H 0.7792 0.4042 0.4065 0.045 Uiso 1 1 calc R . . C10 C 0.7148(6) 0.2656(5) 0.4759(5) 0.0419(16) Uani 1 1 d . . . H10A H 0.7182 0.2118 0.5437 0.050 Uiso 1 1 calc R . . H10B H 0.6309 0.2962 0.4628 0.050 Uiso 1 1 calc R . . C11 C 0.5791(6) 0.4692(6) 0.2483(5) 0.0437(17) Uani 1 1 d . . . C12 C 0.4541(7) 0.5049(8) 0.2150(7) 0.076(3) Uani 1 1 d . . . H12A H 0.4154 0.5638 0.2376 0.114 Uiso 1 1 calc R . . H12B H 0.4111 0.4468 0.2444 0.114 Uiso 1 1 calc R . . H12C H 0.4546 0.5273 0.1415 0.114 Uiso 1 1 calc R . . C13 C 0.8839(6) 0.1453(6) 0.4299(5) 0.0468(17) Uani 1 1 d . . . H13A H 0.8727 0.0769 0.4800 0.056 Uiso 1 1 calc R . . H13B H 0.9265 0.1797 0.4614 0.056 Uiso 1 1 calc R . . C14 C 0.9562(6) 0.1278(5) 0.3379(5) 0.0434(16) Uani 1 1 d . . . H14A H 1.0360 0.0883 0.3579 0.052 Uiso 1 1 calc R . . H14B H 0.9185 0.0855 0.3118 0.052 Uiso 1 1 calc R . . C15 C 1.0493(6) 0.2849(6) 0.2819(6) 0.0498(18) Uani 1 1 d . . . H15A H 1.0468 0.2697 0.3555 0.060 Uiso 1 1 calc R . . H15B H 1.1304 0.2592 0.2600 0.060 Uiso 1 1 calc R . . C16 C 1.0166(6) 0.4010(6) 0.2299(5) 0.0463(17) Uani 1 1 d . . . C17 C 1.0988(7) 0.4678(7) 0.2044(7) 0.063(2) Uani 1 1 d . . . H17A H 1.1798 0.4399 0.2155 0.076 Uiso 1 1 calc R . . C18 C 1.0607(8) 0.5737(7) 0.1633(7) 0.072(3) Uani 1 1 d . . . H18A H 1.1153 0.6195 0.1492 0.086 Uiso 1 1 calc R . . C19 C 0.9443(8) 0.6151(6) 0.1419(6) 0.061(2) Uani 1 1 d . . . H19A H 0.9185 0.6884 0.1112 0.073 Uiso 1 1 calc R . . C20 C 0.8651(7) 0.5450(5) 0.1671(5) 0.0502(18) Uani 1 1 d . . . H20A H 0.7848 0.5718 0.1525 0.060 Uiso 1 1 calc R . . C21 C 1.0020(6) 0.2135(6) 0.1581(5) 0.0488(18) Uani 1 1 d . . . H21A H 1.0616 0.1484 0.1683 0.059 Uiso 1 1 calc R . . H21B H 1.0383 0.2729 0.1132 0.059 Uiso 1 1 calc R . . C22 C 0.8977(6) 0.2060(5) 0.1084(5) 0.0432(17) Uani 1 1 d . . . C23 C 0.9067(7) 0.1537(6) 0.0400(6) 0.058(2) Uani 1 1 d . . . H23A H 0.9805 0.1160 0.0245 0.069 Uiso 1 1 calc R . . C24 C 0.8068(8) 0.1571(7) -0.0056(6) 0.062(2) Uani 1 1 d . . . H24A H 0.8112 0.1216 -0.0526 0.074 Uiso 1 1 calc R . . C25 C 0.7001(7) 0.2131(7) 0.0182(6) 0.062(2) Uani 1 1 d . . . H25A H 0.6309 0.2175 -0.0132 0.074 Uiso 1 1 calc R . . C26 C 0.6961(7) 0.2624(6) 0.0887(6) 0.056(2) Uani 1 1 d . . . H26A H 0.6230 0.3001 0.1054 0.067 Uiso 1 1 calc R . . C27 C 0.6823(6) 0.1504(6) 0.3850(5) 0.0492(18) Uani 1 1 d . . . H27A H 0.6404 0.1727 0.3255 0.059 Uiso 1 1 calc R . . C28 C 0.6675(6) 0.0493(6) 0.4716(5) 0.0445(17) Uani 1 1 d . . . C29 C 0.7231(7) -0.0485(7) 0.4639(7) 0.062(2) Uani 1 1 d . . . H29A H 0.7706 -0.0506 0.4052 0.074 Uiso 1 1 calc R . . C30 C 0.7106(8) -0.1422(7) 0.5398(7) 0.067(2) Uani 1 1 d . . . H30A H 0.7494 -0.2071 0.5324 0.081 Uiso 1 1 calc R . . C31 C 0.6417(8) -0.1414(7) 0.6263(6) 0.067(2) Uani 1 1 d . . . H31A H 0.6332 -0.2052 0.6783 0.080 Uiso 1 1 calc R . . C32 C 0.5855(7) -0.0460(6) 0.6359(6) 0.058(2) Uani 1 1 d . . . H32A H 0.5395 -0.0442 0.6954 0.070 Uiso 1 1 calc R . . C33 C 0.5966(7) 0.0477(6) 0.5577(6) 0.057(2) Uani 1 1 d . . . H33A H 0.5544 0.1122 0.5639 0.069 Uiso 1 1 calc R . . F1 F 0.9657(5) -0.2338(5) 0.3552(5) 0.115(2) Uani 1 1 d . . . F2 F 1.0796(5) -0.1173(5) 0.3416(4) 0.1015(19) Uani 1 1 d . . . F3 F 1.0718(5) -0.0591(4) 0.1759(4) 0.0818(16) Uani 1 1 d . . . F4 F 1.1326(4) -0.2320(4) 0.2561(4) 0.0832(16) Uani 1 1 d . . . F5 F 0.9029(4) -0.0613(4) 0.2690(4) 0.0853(16) Uani 1 1 d . . . F6 F 0.9552(4) -0.1762(4) 0.1874(4) 0.0809(15) Uani 1 1 d . . . F7 F 0.2503(6) 0.2072(7) -0.0174(7) 0.149(3) Uani 1 1 d . . . F8 F 0.3932(6) 0.3025(5) -0.0468(6) 0.152(4) Uani 1 1 d . . . F9 F 0.4282(6) 0.2354(8) 0.1163(6) 0.152(3) Uani 1 1 d . . . F10 F 0.2404(5) 0.3178(5) 0.0627(6) 0.113(2) Uani 1 1 d . . . F11 F 0.2880(5) 0.1433(5) 0.1433(5) 0.126(3) Uani 1 1 d . . . F12 F 0.4355(5) 0.1293(5) 0.0286(5) 0.1018(19) 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 Cu1 0.0274(4) 0.0400(5) 0.0517(5) -0.0163(4) 0.0005(4) -0.0010(3) Cu2 0.0221(4) 0.0284(4) 0.0439(5) -0.0059(3) 0.0031(3) -0.0043(3) P1 0.0393(10) 0.0510(12) 0.0539(11) -0.0154(9) -0.0017(9) -0.0113(9) P2 0.0456(13) 0.0738(16) 0.0740(16) -0.0041(13) 0.0053(11) -0.0021(11) N1 0.033(3) 0.032(3) 0.047(3) -0.007(3) 0.001(2) -0.008(2) N2 0.038(3) 0.026(3) 0.055(4) 0.000(3) -0.003(3) -0.005(2) N3 0.022(3) 0.031(3) 0.052(3) -0.011(2) 0.004(2) 0.000(2) N4 0.027(3) 0.040(3) 0.051(3) -0.015(3) 0.001(2) -0.007(2) N5 0.027(3) 0.039(3) 0.057(4) -0.015(3) 0.002(3) -0.003(2) N6 0.029(3) 0.033(3) 0.052(3) -0.012(3) 0.000(2) -0.002(2) N7 0.035(3) 0.053(4) 0.048(3) -0.022(3) 0.002(3) -0.011(3) O1 0.018(2) 0.035(2) 0.042(2) -0.0024(19) 0.0038(18) 0.0001(18) O2 0.043(3) 0.051(3) 0.056(3) -0.019(3) 0.003(2) 0.002(2) O3 0.034(3) 0.061(3) 0.077(4) -0.037(3) -0.006(2) 0.008(2) C1 0.025(3) 0.034(4) 0.062(5) -0.007(3) -0.004(3) -0.009(3) C2 0.029(3) 0.029(3) 0.053(4) -0.010(3) 0.003(3) -0.005(3) C3 0.040(4) 0.037(4) 0.046(4) -0.001(3) 0.001(3) -0.001(3) C4 0.030(4) 0.042(4) 0.051(4) -0.008(3) -0.004(3) -0.002(3) C5 0.048(4) 0.032(4) 0.074(5) 0.006(4) -0.003(4) -0.014(3) C6 0.021(3) 0.036(4) 0.072(5) -0.007(3) -0.006(3) -0.007(3) C7 0.032(4) 0.042(4) 0.062(5) -0.009(3) -0.009(3) -0.009(3) C8 0.020(3) 0.036(4) 0.049(4) -0.013(3) 0.001(3) -0.003(3) C9 0.026(3) 0.035(4) 0.047(4) -0.011(3) 0.001(3) -0.001(3) C10 0.036(4) 0.041(4) 0.052(4) -0.023(3) 0.013(3) -0.009(3) C11 0.038(4) 0.049(4) 0.042(4) -0.014(3) -0.003(3) -0.004(3) C12 0.040(5) 0.093(7) 0.092(7) -0.040(6) -0.013(4) 0.015(5) C13 0.041(4) 0.037(4) 0.053(4) -0.009(3) -0.001(3) 0.001(3) C14 0.042(4) 0.027(3) 0.053(4) -0.011(3) 0.000(3) 0.005(3) C15 0.032(4) 0.046(4) 0.067(5) -0.014(4) -0.009(3) -0.004(3) C16 0.040(4) 0.051(4) 0.052(4) -0.021(3) -0.003(3) -0.011(3) C17 0.044(5) 0.060(6) 0.086(6) -0.018(5) -0.008(4) -0.016(4) C18 0.059(6) 0.055(6) 0.105(7) -0.021(5) -0.010(5) -0.023(4) C19 0.069(6) 0.037(4) 0.073(6) -0.009(4) -0.008(4) -0.012(4) C20 0.048(4) 0.041(4) 0.056(5) -0.013(3) -0.003(4) -0.002(3) C21 0.039(4) 0.048(4) 0.054(4) -0.017(3) 0.013(3) -0.004(3) C22 0.037(4) 0.039(4) 0.051(4) -0.016(3) 0.014(3) -0.008(3) C23 0.050(5) 0.060(5) 0.058(5) -0.022(4) 0.013(4) -0.004(4) C24 0.082(6) 0.063(5) 0.050(5) -0.030(4) 0.007(4) -0.021(5) C25 0.054(5) 0.083(6) 0.059(5) -0.029(5) -0.004(4) -0.024(5) C26 0.049(5) 0.064(5) 0.058(5) -0.023(4) 0.000(4) -0.015(4) C27 0.049(4) 0.049(4) 0.048(4) -0.008(3) -0.007(3) -0.016(4) C28 0.040(4) 0.046(4) 0.057(4) -0.028(4) 0.010(3) -0.017(3) C29 0.055(5) 0.066(6) 0.067(5) -0.027(5) 0.009(4) -0.014(4) C30 0.063(6) 0.047(5) 0.086(7) -0.016(5) -0.016(5) -0.005(4) C31 0.074(6) 0.060(6) 0.059(5) 0.000(4) -0.009(5) -0.026(5) C32 0.066(5) 0.059(5) 0.051(5) -0.018(4) 0.004(4) -0.021(4) C33 0.051(5) 0.052(5) 0.070(5) -0.023(4) 0.006(4) -0.014(4) F1 0.090(4) 0.119(5) 0.108(5) 0.016(4) 0.003(3) -0.059(4) F2 0.109(5) 0.132(5) 0.085(4) -0.037(4) -0.030(3) -0.051(4) F3 0.092(4) 0.060(3) 0.078(3) -0.008(3) 0.014(3) -0.016(3) F4 0.048(3) 0.061(3) 0.132(5) -0.025(3) -0.020(3) 0.007(2) F5 0.062(3) 0.101(4) 0.110(4) -0.073(4) 0.002(3) 0.010(3) F6 0.065(3) 0.096(4) 0.107(4) -0.066(3) -0.026(3) -0.001(3) F7 0.103(5) 0.173(7) 0.186(8) -0.093(6) -0.072(5) 0.033(5) F8 0.108(5) 0.109(5) 0.137(6) 0.037(4) 0.067(5) 0.019(4) F9 0.080(5) 0.254(10) 0.146(6) -0.085(7) 0.003(4) -0.057(6) F10 0.069(4) 0.094(4) 0.165(6) -0.048(4) 0.043(4) -0.007(3) F11 0.060(4) 0.128(5) 0.128(5) 0.025(4) 0.016(3) -0.010(3) F12 0.073(4) 0.086(4) 0.111(4) -0.010(3) -0.006(3) 0.018(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 Cu1 O3 1.914(5) . ? Cu1 N5 2.045(5) . ? Cu1 N6 2.079(5) . ? Cu1 N7 2.079(6) . ? Cu1 N4 2.187(5) . ? Cu2 O1 1.924(4) 2_666 ? Cu2 O1 1.933(4) . ? Cu2 N3 2.011(5) . ? Cu2 N1 2.019(5) . ? Cu2 O2 2.243(5) . ? Cu2 Cu2 3.0154(14) 2_666 ? P1 F2 1.570(5) . ? P1 F1 1.572(5) . ? P1 F3 1.573(5) . ? P1 F4 1.573(5) . ? P1 F6 1.578(5) . ? P1 F5 1.596(5) . ? P2 F8 1.537(6) . ? P2 F9 1.552(8) . ? P2 F7 1.565(7) . ? P2 F11 1.572(6) . ? P2 F12 1.587(6) . ? P2 F10 1.587(6) . ? N1 C1 1.267(8) . ? N1 C6 1.476(8) . ? N2 C2 1.343(8) . ? N2 C3 1.381(9) . ? N2 C5 1.475(8) . ? N3 C2 1.331(8) . ? N3 C4 1.370(8) . ? N4 C13 1.485(8) . ? N4 C27 1.495(9) . ? N4 C10 1.504(8) . ? N5 C14 1.470(8) . ? N5 C15 1.485(9) . ? N5 C21 1.490(9) . ? N6 C16 1.347(9) . ? N6 C20 1.350(8) . ? N7 C26 1.325(9) . ? N7 C22 1.351(8) . ? O1 C8 1.431(7) 2_666 ? O1 Cu2 1.924(4) 2_666 ? O2 C11 1.212(8) . ? O3 C11 1.278(8) . ? C1 C2 1.451(9) . ? C3 C4 1.368(9) . ? C6 C7 1.527(9) . ? C7 C8 1.532(9) . ? C8 O1 1.431(7) 2_666 ? C8 C9 1.522(9) . ? C9 C10 1.524(9) . ? C11 C12 1.497(10) . ? C13 C14 1.515(9) . ? C15 C16 1.485(10) . ? C16 C17 1.389(10) . ? C17 C18 1.354(11) . ? C18 C19 1.366(12) . ? C19 C20 1.396(10) . ? C21 C22 1.502(10) . ? C22 C23 1.371(10) . ? C23 C24 1.371(11) . ? C24 C25 1.374(11) . ? C25 C26 1.374(11) . ? C27 C28 1.518(10) . ? C28 C33 1.374(10) . ? C28 C29 1.390(10) . ? C29 C30 1.377(11) . ? C30 C31 1.373(12) . ? C31 C32 1.373(12) . ? C32 C33 1.388(11) . ? 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 O3 Cu1 N5 168.7(2) . . ? O3 Cu1 N6 107.0(2) . . ? N5 Cu1 N6 81.0(2) . . ? O3 Cu1 N7 87.8(2) . . ? N5 Cu1 N7 81.4(2) . . ? N6 Cu1 N7 116.9(2) . . ? O3 Cu1 N4 96.9(2) . . ? N5 Cu1 N4 84.3(2) . . ? N6 Cu1 N4 125.3(2) . . ? N7 Cu1 N4 112.4(2) . . ? O1 Cu2 O1 77.16(18) 2_666 . ? O1 Cu2 N3 170.3(2) 2_666 . ? O1 Cu2 N3 104.46(18) . . ? O1 Cu2 N1 93.55(19) 2_666 . ? O1 Cu2 N1 163.0(2) . . ? N3 Cu2 N1 82.4(2) . . ? O1 Cu2 O2 94.82(18) 2_666 . ? O1 Cu2 O2 107.87(19) . . ? N3 Cu2 O2 93.7(2) . . ? N1 Cu2 O2 86.9(2) . . ? O1 Cu2 Cu2 38.69(11) 2_666 2_666 ? O1 Cu2 Cu2 38.48(12) . 2_666 ? N3 Cu2 Cu2 142.11(14) . 2_666 ? N1 Cu2 Cu2 130.73(16) . 2_666 ? O2 Cu2 Cu2 104.50(13) . 2_666 ? F2 P1 F1 90.1(4) . . ? F2 P1 F3 88.4(3) . . ? F1 P1 F3 178.2(4) . . ? F2 P1 F4 91.0(3) . . ? F1 P1 F4 90.6(3) . . ? F3 P1 F4 90.4(3) . . ? F2 P1 F6 178.6(4) . . ? F1 P1 F6 89.8(3) . . ? F3 P1 F6 91.6(3) . . ? F4 P1 F6 90.4(3) . . ? F2 P1 F5 90.7(3) . . ? F1 P1 F5 90.4(3) . . ? F3 P1 F5 88.5(3) . . ? F4 P1 F5 178.0(3) . . ? F6 P1 F5 87.9(3) . . ? F8 P2 F9 91.2(5) . . ? F8 P2 F7 92.1(5) . . ? F9 P2 F7 176.6(5) . . ? F8 P2 F11 179.3(4) . . ? F9 P2 F11 88.5(4) . . ? F7 P2 F11 88.2(5) . . ? F8 P2 F12 89.8(3) . . ? F9 P2 F12 88.8(4) . . ? F7 P2 F12 90.3(4) . . ? F11 P2 F12 89.5(3) . . ? F8 P2 F10 90.6(4) . . ? F9 P2 F10 94.2(5) . . ? F7 P2 F10 86.6(4) . . ? F11 P2 F10 90.1(3) . . ? F12 P2 F10 176.9(4) . . ? C1 N1 C6 119.6(5) . . ? C1 N1 Cu2 113.4(4) . . ? C6 N1 Cu2 126.7(4) . . ? C2 N2 C3 107.2(5) . . ? C2 N2 C5 127.7(6) . . ? C3 N2 C5 125.1(5) . . ? C2 N3 C4 106.2(5) . . ? C2 N3 Cu2 108.8(4) . . ? C4 N3 Cu2 144.7(5) . . ? C13 N4 C27 111.6(5) . . ? C13 N4 C10 110.1(5) . . ? C27 N4 C10 110.3(5) . . ? C13 N4 Cu1 105.1(4) . . ? C27 N4 Cu1 104.9(4) . . ? C10 N4 Cu1 114.6(4) . . ? C14 N5 C15 112.2(6) . . ? C14 N5 C21 110.7(5) . . ? C15 N5 C21 110.1(5) . . ? C14 N5 Cu1 106.9(4) . . ? C15 N5 Cu1 108.6(4) . . ? C21 N5 Cu1 108.1(4) . . ? C16 N6 C20 119.0(6) . . ? C16 N6 Cu1 113.2(4) . . ? C20 N6 Cu1 127.6(5) . . ? C26 N7 C22 119.1(6) . . ? C26 N7 Cu1 126.8(5) . . ? C22 N7 Cu1 114.0(5) . . ? C8 O1 Cu2 125.3(3) 2_666 2_666 ? C8 O1 Cu2 131.4(4) 2_666 . ? Cu2 O1 Cu2 102.83(18) 2_666 . ? C11 O2 Cu2 136.1(5) . . ? C11 O3 Cu1 128.9(5) . . ? N1 C1 C2 115.4(6) . . ? N3 C2 N2 111.1(6) . . ? N3 C2 C1 119.7(6) . . ? N2 C2 C1 129.1(6) . . ? C4 C3 N2 106.1(6) . . ? C3 C4 N3 109.3(6) . . ? N1 C6 C7 110.4(5) . . ? C6 C7 C8 115.8(6) . . ? O1 C8 C9 112.4(5) 2_666 . ? O1 C8 C7 109.7(5) 2_666 . ? C9 C8 C7 111.1(5) . . ? C8 C9 C10 113.3(5) . . ? N4 C10 C9 113.9(5) . . ? O2 C11 O3 124.1(7) . . ? O2 C11 C12 121.3(7) . . ? O3 C11 C12 114.6(7) . . ? N4 C13 C14 109.9(6) . . ? N5 C14 C13 110.9(5) . . ? C16 C15 N5 110.2(6) . . ? N6 C16 C17 121.1(7) . . ? N6 C16 C15 116.2(6) . . ? C17 C16 C15 122.6(7) . . ? C18 C17 C16 119.1(8) . . ? C17 C18 C19 121.2(8) . . ? C18 C19 C20 117.7(7) . . ? N6 C20 C19 121.8(7) . . ? N5 C21 C22 111.4(5) . . ? N7 C22 C23 121.4(7) . . ? N7 C22 C21 114.7(6) . . ? C23 C22 C21 123.9(6) . . ? C22 C23 C24 119.2(7) . . ? C23 C24 C25 119.2(8) . . ? C26 C25 C24 119.0(8) . . ? N7 C26 C25 122.0(8) . . ? N4 C27 C28 116.9(6) . . ? C33 C28 C29 116.7(7) . . ? C33 C28 C27 123.4(7) . . ? C29 C28 C27 119.9(6) . . ? C30 C29 C28 121.9(8) . . ? C31 C30 C29 120.2(8) . . ? C30 C31 C32 119.1(8) . . ? C31 C32 C33 120.0(8) . . ? C28 C33 C32 122.0(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.685 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.098 #===END data_complex_9 _database_code_CSD 170796 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H92 Cu4 F12 N10 O10 P2' _chemical_formula_weight 1825.68 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' 'Cu' 'Cu' 0.3201 1.2651 '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 10.3158(2) _cell_length_b 12.0891(2) _cell_length_c 17.6124(2) _cell_angle_alpha 74.0125(2) _cell_angle_beta 81.8911(5) _cell_angle_gamma 71.7472(7) _cell_volume 2001.61(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.8913 _exptl_absorpt_process_details 'SADABS, Sheldrick, 98' _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 '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 12766 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7690 _reflns_number_gt 6499 _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^)+(0.1000P)^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 7690 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1922 _refine_ls_goodness_of_fit_ref 1.618 _refine_ls_restrained_S_all 1.618 _refine_ls_shift/su_max 0.006 _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 Cu1 Cu 0.65101(5) 0.43021(5) 0.51172(3) 0.02878(19) Uani 1 1 d . . . Cu2 Cu 0.63216(5) 0.27924(5) 0.27250(3) 0.02837(19) Uani 1 1 d . . . O1 O 0.7292(3) 0.2955(3) 0.5938(2) 0.0405(8) Uani 1 1 d . . . O2 O 0.5328(3) 0.5565(3) 0.43766(19) 0.0304(7) Uani 1 1 d . . . O3 O 0.5992(4) 0.2376(3) 0.3875(2) 0.0466(9) Uani 1 1 d . . . O4 O 0.3867(5) 0.2317(5) 0.4164(3) 0.0756(15) Uani 1 1 d . . . N1 N 0.8275(4) 0.4452(4) 0.4563(2) 0.0344(9) Uani 1 1 d . . . N2 N 0.4725(4) 0.4443(3) 0.2359(2) 0.0278(8) Uani 1 1 d . . . N3 N 0.7009(4) 0.3094(4) 0.1549(2) 0.0375(10) Uani 1 1 d . . . N4 N 0.5880(4) 0.1354(3) 0.2434(2) 0.0325(9) Uani 1 1 d . . . N5 N 0.8367(4) 0.2595(4) 0.2856(3) 0.0348(9) Uani 1 1 d . . . C1 C 0.8611(5) 0.2341(4) 0.6005(3) 0.0359(11) Uani 1 1 d . . . C2 C 0.8972(6) 0.1313(5) 0.6642(3) 0.0418(12) Uani 1 1 d . . . H2A H 0.8280 0.1076 0.7008 0.050 Uiso 1 1 calc R . . C3 C 1.0361(6) 0.0634(5) 0.6736(4) 0.0528(16) Uani 1 1 d . . . H3A H 1.0589 -0.0051 0.7168 0.063 Uiso 1 1 calc R . . C4 C 1.1391(6) 0.0952(5) 0.6209(4) 0.0526(16) Uani 1 1 d . . . H4A H 1.2316 0.0484 0.6277 0.063 Uiso 1 1 calc R . . C5 C 1.1063(5) 0.1946(6) 0.5589(4) 0.0495(14) Uani 1 1 d . . . H5A H 1.1772 0.2158 0.5228 0.059 Uiso 1 1 calc R . . C6 C 0.9677(5) 0.2675(4) 0.5472(3) 0.0362(11) Uani 1 1 d . . . C7 C 0.9442(5) 0.3702(5) 0.4801(3) 0.0383(11) Uani 1 1 d . . . H7A H 1.0234 0.3850 0.4496 0.046 Uiso 1 1 calc R . . C8 C 0.8365(5) 0.5422(5) 0.3824(3) 0.0394(11) Uani 1 1 d . . . H8A H 0.8552 0.5068 0.3361 0.047 Uiso 1 1 calc R . . H8B H 0.9149 0.5715 0.3850 0.047 Uiso 1 1 calc R . . C9 C 0.7076(5) 0.6492(5) 0.3696(3) 0.0391(11) Uani 1 1 d . . . H9A H 0.7241 0.7094 0.3212 0.047 Uiso 1 1 calc R . . H9B H 0.6922 0.6869 0.4146 0.047 Uiso 1 1 calc R . . C10 C 0.5759(5) 0.6194(4) 0.3614(3) 0.0303(10) Uani 1 1 d . . . H10A H 0.5030 0.6969 0.3444 0.036 Uiso 1 1 calc R . . C11 C 0.5942(5) 0.5468(4) 0.2997(3) 0.0297(9) Uani 1 1 d . . . H11A H 0.6313 0.5889 0.2490 0.036 Uiso 1 1 calc R . . H11B H 0.6608 0.4671 0.3176 0.036 Uiso 1 1 calc R . . C12 C 0.4585(5) 0.5302(4) 0.2869(3) 0.0309(10) Uani 1 1 d . . . H12A H 0.4149 0.5002 0.3391 0.037 Uiso 1 1 calc R . . H12B H 0.3969 0.6095 0.2620 0.037 Uiso 1 1 calc R . . C13 C 0.3396(5) 0.4115(4) 0.2417(3) 0.0306(10) Uani 1 1 d . . . H13A H 0.3547 0.3491 0.2122 0.037 Uiso 1 1 calc R . . H13B H 0.3183 0.3754 0.2979 0.037 Uiso 1 1 calc R . . C14 C 0.2154(5) 0.5146(4) 0.2105(3) 0.0326(10) Uani 1 1 d . . . C15 C 0.1732(6) 0.5300(5) 0.1353(3) 0.0484(14) Uani 1 1 d . . . H15A H 0.2252 0.4784 0.1029 0.058 Uiso 1 1 calc R . . C16 C 0.0549(7) 0.6208(6) 0.1069(4) 0.0635(18) Uani 1 1 d . . . H16A H 0.0270 0.6285 0.0561 0.076 Uiso 1 1 calc R . . C17 C -0.0220(6) 0.6996(6) 0.1521(4) 0.0577(16) Uani 1 1 d . . . H17A H -0.1007 0.7618 0.1321 0.069 Uiso 1 1 calc R . . C18 C 0.0192(6) 0.6854(5) 0.2289(4) 0.0476(13) Uani 1 1 d . . . H18A H -0.0320 0.7383 0.2607 0.057 Uiso 1 1 calc R . . C19 C 0.1360(5) 0.5927(5) 0.2574(3) 0.0375(11) Uani 1 1 d . . . H19A H 0.1620 0.5823 0.3091 0.045 Uiso 1 1 calc R . . C20 C 0.5131(6) 0.4972(4) 0.1517(3) 0.0357(11) Uani 1 1 d . . . H20A H 0.5764 0.5446 0.1506 0.043 Uiso 1 1 calc R . . H20B H 0.4309 0.5519 0.1241 0.043 Uiso 1 1 calc R . . C21 C 0.5824(6) 0.3980(5) 0.1094(3) 0.0383(11) Uani 1 1 d . . . H21A H 0.5159 0.3564 0.1050 0.046 Uiso 1 1 calc R . . H21B H 0.6154 0.4330 0.0553 0.046 Uiso 1 1 calc R . . C22 C 0.7432(6) 0.1928(5) 0.1316(3) 0.0472(14) Uani 1 1 d . . . H22A H 0.8395 0.1502 0.1443 0.057 Uiso 1 1 calc R . . H22B H 0.7377 0.2087 0.0738 0.057 Uiso 1 1 calc R . . C23 C 0.6540(6) 0.1133(4) 0.1738(3) 0.0415(12) Uani 1 1 d . . . C24 C 0.6432(7) 0.0192(5) 0.1454(4) 0.0526(15) Uani 1 1 d . . . H24A H 0.6909 0.0045 0.0973 0.063 Uiso 1 1 calc R . . C25 C 0.5631(7) -0.0514(5) 0.1877(4) 0.0597(17) Uani 1 1 d . . . H25A H 0.5550 -0.1156 0.1692 0.072 Uiso 1 1 calc R . . C26 C 0.4925(6) -0.0276(5) 0.2593(4) 0.0485(14) Uani 1 1 d . . . H26A H 0.4354 -0.0745 0.2890 0.058 Uiso 1 1 calc R . . C27 C 0.5085(5) 0.0652(4) 0.2848(3) 0.0370(11) Uani 1 1 d . . . H27A H 0.4622 0.0807 0.3330 0.044 Uiso 1 1 calc R . . C28 C 0.8230(6) 0.3557(5) 0.1457(3) 0.0465(13) Uani 1 1 d . . . H28A H 0.7921 0.4434 0.1410 0.056 Uiso 1 1 calc R . . H28B H 0.8785 0.3410 0.0969 0.056 Uiso 1 1 calc R . . C29 C 0.9093(5) 0.2929(5) 0.2168(4) 0.0435(12) Uani 1 1 d . . . C30 C 1.0504(6) 0.2728(6) 0.2127(5) 0.0608(18) Uani 1 1 d . . . H30A H 1.0992 0.2960 0.1640 0.073 Uiso 1 1 calc R . . C31 C 1.1176(6) 0.2173(7) 0.2830(6) 0.074(2) Uani 1 1 d . . . H31A H 1.2141 0.2002 0.2822 0.088 Uiso 1 1 calc R . . C32 C 1.0456(6) 0.1875(5) 0.3525(4) 0.0523(15) Uani 1 1 d . . . H32A H 1.0911 0.1533 0.4004 0.063 Uiso 1 1 calc R . . C33 C 0.9048(5) 0.2071(5) 0.3533(4) 0.0418(12) Uani 1 1 d . . . H33A H 0.8556 0.1835 0.4018 0.050 Uiso 1 1 calc R . . C34 C 0.5077(6) 0.2117(5) 0.4323(3) 0.0426(12) Uani 1 1 d . . . C35 C 0.5492(7) 0.1387(5) 0.5173(3) 0.0536(15) Uani 1 1 d . . . H35A H 0.6469 0.1257 0.5212 0.080 Uiso 1 1 calc R . . H35B H 0.5305 0.0609 0.5285 0.080 Uiso 1 1 calc R . . H35C H 0.4962 0.1835 0.5556 0.080 Uiso 1 1 calc R . . P1 P 0.33343(14) 0.24856(12) 0.00401(8) 0.0375(3) Uani 1 1 d . . . F1 F 0.1897(5) 0.2297(8) 0.0148(3) 0.156(3) Uani 1 1 d . . . F2 F 0.4055(7) 0.1104(4) 0.0131(3) 0.118(2) Uani 1 1 d . . . F3 F 0.4810(5) 0.2671(6) -0.0068(3) 0.110(2) Uani 1 1 d . . . F4 F 0.2708(8) 0.3875(4) -0.0061(3) 0.132(3) Uani 1 1 d . . . F5 F 0.3360(3) 0.2276(3) 0.09854(18) 0.0550(9) Uani 1 1 d . . . F6 F 0.3316(5) 0.2733(4) -0.0905(2) 0.0687(11) Uani 1 1 d . . . O5 O 0.7488(11) 0.1234(10) -0.1052(6) 0.173(4) Uani 1 1 d . . . H5B H 0.7441 0.1721 -0.0782 0.259 Uiso 1 1 calc R . . C50 C 0.9238(19) -0.0396(13) -0.1326(12) 0.315(19) Uani 1 1 d . . . H50A H 1.0188 -0.0824 -0.1197 0.473 Uiso 1 1 calc R . . H50B H 0.9195 -0.0088 -0.1901 0.473 Uiso 1 1 calc R . . H50C H 0.8675 -0.0949 -0.1136 0.473 Uiso 1 1 calc R . . C51 C 0.8832(15) 0.0397(8) -0.1026(9) 0.154(7) Uani 1 1 d . . . H51B H 0.9468 0.0895 -0.1221 0.184 Uiso 1 1 calc R . . H51A H 0.8985 0.0037 -0.0457 0.184 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0217(3) 0.0313(3) 0.0332(3) -0.0124(2) -0.0054(2) -0.0021(2) Cu2 0.0293(3) 0.0319(3) 0.0218(3) -0.0041(2) -0.0003(2) -0.0087(2) O1 0.0245(16) 0.044(2) 0.043(2) -0.0080(16) -0.0060(14) 0.0020(15) O2 0.0251(15) 0.0338(17) 0.0297(17) -0.0082(13) -0.0034(13) -0.0036(13) O3 0.065(3) 0.048(2) 0.0275(18) 0.0030(15) -0.0151(18) -0.0211(19) O4 0.056(3) 0.107(4) 0.044(3) 0.007(3) 0.005(2) -0.021(3) N1 0.026(2) 0.039(2) 0.041(2) -0.0162(18) -0.0038(17) -0.0067(17) N2 0.033(2) 0.0289(19) 0.0209(18) -0.0038(14) -0.0016(15) -0.0094(16) N3 0.043(2) 0.034(2) 0.028(2) -0.0057(17) 0.0073(17) -0.0069(19) N4 0.037(2) 0.0262(19) 0.032(2) -0.0028(15) -0.0094(17) -0.0059(17) N5 0.032(2) 0.033(2) 0.040(2) -0.0131(17) -0.0012(17) -0.0078(17) C1 0.032(2) 0.031(2) 0.046(3) -0.017(2) -0.011(2) -0.002(2) C2 0.042(3) 0.037(3) 0.046(3) -0.012(2) -0.016(2) -0.003(2) C3 0.054(4) 0.034(3) 0.073(4) -0.022(3) -0.029(3) 0.004(3) C4 0.035(3) 0.041(3) 0.080(4) -0.027(3) -0.028(3) 0.011(2) C5 0.030(3) 0.055(3) 0.070(4) -0.030(3) -0.013(3) -0.004(2) C6 0.026(2) 0.037(3) 0.049(3) -0.024(2) -0.012(2) 0.002(2) C7 0.025(2) 0.045(3) 0.051(3) -0.027(2) 0.000(2) -0.008(2) C8 0.033(3) 0.044(3) 0.047(3) -0.013(2) -0.001(2) -0.019(2) C9 0.036(3) 0.037(3) 0.050(3) -0.010(2) -0.007(2) -0.017(2) C10 0.029(2) 0.027(2) 0.033(2) -0.0053(18) -0.0031(18) -0.0075(19) C11 0.028(2) 0.032(2) 0.030(2) -0.0087(18) -0.0023(18) -0.0082(18) C12 0.037(2) 0.030(2) 0.026(2) -0.0077(18) -0.0033(18) -0.0074(19) C13 0.032(2) 0.030(2) 0.033(2) -0.0079(19) -0.0067(19) -0.011(2) C14 0.041(3) 0.031(2) 0.029(2) -0.0065(19) -0.010(2) -0.012(2) C15 0.052(3) 0.051(3) 0.042(3) -0.021(3) -0.015(3) -0.002(3) C16 0.063(4) 0.070(4) 0.050(4) -0.016(3) -0.030(3) 0.003(3) C17 0.039(3) 0.049(3) 0.077(4) -0.014(3) -0.019(3) 0.004(3) C18 0.034(3) 0.048(3) 0.063(4) -0.022(3) -0.006(2) -0.006(2) C19 0.033(2) 0.044(3) 0.038(3) -0.016(2) -0.002(2) -0.009(2) C20 0.049(3) 0.033(2) 0.023(2) -0.0027(19) 0.000(2) -0.015(2) C21 0.055(3) 0.038(3) 0.019(2) -0.0013(19) -0.004(2) -0.013(2) C22 0.058(3) 0.040(3) 0.035(3) -0.015(2) 0.009(2) -0.002(3) C23 0.053(3) 0.031(2) 0.037(3) -0.011(2) -0.013(2) 0.000(2) C24 0.074(4) 0.038(3) 0.042(3) -0.020(2) -0.009(3) 0.001(3) C25 0.078(5) 0.032(3) 0.071(4) -0.017(3) -0.023(4) -0.007(3) C26 0.057(3) 0.028(3) 0.060(4) -0.002(2) -0.021(3) -0.012(2) C27 0.040(3) 0.028(2) 0.041(3) -0.002(2) -0.017(2) -0.006(2) C28 0.043(3) 0.049(3) 0.041(3) -0.005(2) 0.013(2) -0.015(3) C29 0.035(3) 0.041(3) 0.057(3) -0.018(2) 0.011(2) -0.015(2) C30 0.033(3) 0.052(4) 0.096(5) -0.023(3) 0.016(3) -0.014(3) C31 0.028(3) 0.065(4) 0.133(7) -0.034(5) -0.004(4) -0.011(3) C32 0.039(3) 0.044(3) 0.080(5) -0.028(3) -0.015(3) -0.004(2) C33 0.033(3) 0.036(3) 0.058(3) -0.021(2) -0.011(2) 0.000(2) C34 0.039(3) 0.045(3) 0.043(3) -0.022(2) -0.003(2) -0.002(2) C35 0.073(4) 0.047(3) 0.034(3) -0.006(2) 0.005(3) -0.015(3) P1 0.0461(8) 0.0346(7) 0.0316(7) -0.0080(5) -0.0009(5) -0.0121(6) F1 0.086(4) 0.306(9) 0.070(3) 0.059(4) -0.037(3) -0.124(5) F2 0.194(6) 0.056(3) 0.094(4) -0.032(3) -0.033(4) 0.001(3) F3 0.087(3) 0.208(6) 0.049(2) -0.009(3) -0.001(2) -0.080(4) F4 0.260(8) 0.040(2) 0.050(3) -0.0100(19) -0.005(4) 0.019(3) F5 0.0510(19) 0.068(2) 0.0297(16) -0.0025(15) -0.0012(14) -0.0032(17) F6 0.098(3) 0.089(3) 0.0363(19) -0.0167(18) -0.0057(19) -0.049(2) O5 0.154(9) 0.177(10) 0.161(9) -0.043(8) 0.032(7) -0.029(7) C50 0.246(19) 0.104(10) 0.33(3) 0.080(13) 0.22(2) 0.096(12) C51 0.158(12) 0.050(5) 0.214(15) -0.027(7) 0.100(11) -0.028(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.898(4) . ? Cu1 O2 1.925(3) . ? Cu1 O2 1.956(3) 2_666 ? Cu1 N1 1.977(4) . ? Cu2 O3 1.956(4) . ? Cu2 N3 2.063(4) . ? Cu2 N5 2.086(4) . ? Cu2 N4 2.133(4) . ? Cu2 N2 2.154(4) . ? O1 C1 1.334(6) . ? O2 C10 1.435(6) . ? O2 Cu1 1.956(3) 2_666 ? O3 C34 1.203(7) . ? O4 C34 1.252(7) . ? N1 C7 1.302(6) . ? N1 C8 1.507(7) . ? N2 C20 1.501(6) . ? N2 C12 1.513(6) . ? N2 C13 1.526(6) . ? N3 C22 1.493(6) . ? N3 C28 1.503(7) . ? N3 C21 1.506(6) . ? N4 C27 1.360(7) . ? N4 C23 1.366(7) . ? N5 C33 1.362(7) . ? N5 C29 1.363(7) . ? C1 C2 1.415(7) . ? C1 C6 1.425(8) . ? C2 C3 1.417(7) . ? C3 C4 1.385(10) . ? C4 C5 1.370(9) . ? C5 C6 1.435(7) . ? C6 C7 1.443(8) . ? C8 C9 1.529(7) . ? C9 C10 1.545(6) . ? C10 C11 1.533(6) . ? C11 C12 1.530(6) . ? C13 C14 1.522(6) . ? C14 C15 1.397(7) . ? C14 C19 1.415(7) . ? C15 C16 1.405(8) . ? C16 C17 1.391(9) . ? C17 C18 1.424(9) . ? C18 C19 1.405(7) . ? C20 C21 1.521(7) . ? C22 C23 1.514(8) . ? C23 C24 1.403(8) . ? C24 C25 1.372(10) . ? C25 C26 1.419(10) . ? C26 C27 1.378(7) . ? C28 C29 1.518(8) . ? C29 C30 1.393(8) . ? C30 C31 1.398(11) . ? C31 C32 1.359(11) . ? C32 C33 1.396(8) . ? C34 C35 1.555(8) . ? P1 F1 1.547(4) . ? P1 F4 1.568(4) . ? P1 F2 1.574(5) . ? P1 F3 1.585(5) . ? P1 F6 1.610(4) . ? P1 F5 1.616(3) . ? O5 C51 1.435(15) . ? C50 C51 1.16(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 166.48(15) . . ? O1 Cu1 O2 91.77(14) . 2_666 ? O2 Cu1 O2 75.56(15) . 2_666 ? O1 Cu1 N1 95.38(16) . . ? O2 Cu1 N1 97.72(16) . . ? O2 Cu1 N1 170.83(15) 2_666 . ? O3 Cu2 N3 170.43(17) . . ? O3 Cu2 N5 90.15(17) . . ? N3 Cu2 N5 80.85(18) . . ? O3 Cu2 N4 100.42(16) . . ? N3 Cu2 N4 81.01(16) . . ? N5 Cu2 N4 117.05(15) . . ? O3 Cu2 N2 102.90(16) . . ? N3 Cu2 N2 85.29(15) . . ? N5 Cu2 N2 127.46(15) . . ? N4 Cu2 N2 110.25(14) . . ? C1 O1 Cu1 127.4(3) . . ? C10 O2 Cu1 125.5(3) . . ? C10 O2 Cu1 130.0(3) . 2_666 ? Cu1 O2 Cu1 104.44(15) . 2_666 ? C34 O3 Cu2 135.1(4) . . ? C7 N1 C8 115.2(4) . . ? C7 N1 Cu1 122.3(4) . . ? C8 N1 Cu1 122.5(3) . . ? C20 N2 C12 110.7(3) . . ? C20 N2 C13 111.3(4) . . ? C12 N2 C13 110.1(3) . . ? C20 N2 Cu2 105.3(3) . . ? C12 N2 Cu2 112.0(3) . . ? C13 N2 Cu2 107.3(3) . . ? C22 N3 C28 109.1(4) . . ? C22 N3 C21 111.3(4) . . ? C28 N3 C21 113.1(4) . . ? C22 N3 Cu2 108.5(3) . . ? C28 N3 Cu2 108.4(3) . . ? C21 N3 Cu2 106.2(3) . . ? C27 N4 C23 118.7(4) . . ? C27 N4 Cu2 129.1(3) . . ? C23 N4 Cu2 112.2(3) . . ? C33 N5 C29 118.4(5) . . ? C33 N5 Cu2 126.6(4) . . ? C29 N5 Cu2 114.6(4) . . ? O1 C1 C2 118.3(5) . . ? O1 C1 C6 123.4(5) . . ? C2 C1 C6 118.3(5) . . ? C1 C2 C3 120.2(6) . . ? C4 C3 C2 121.2(6) . . ? C5 C4 C3 119.4(5) . . ? C4 C5 C6 121.7(6) . . ? C1 C6 C5 119.1(5) . . ? C1 C6 C7 123.6(4) . . ? C5 C6 C7 117.3(5) . . ? N1 C7 C6 127.8(5) . . ? N1 C8 C9 114.1(4) . . ? C8 C9 C10 115.4(4) . . ? O2 C10 C11 111.1(4) . . ? O2 C10 C9 108.6(4) . . ? C11 C10 C9 112.7(4) . . ? C12 C11 C10 111.4(4) . . ? N2 C12 C11 114.0(4) . . ? C14 C13 N2 115.9(4) . . ? C15 C14 C19 118.3(5) . . ? C15 C14 C13 120.0(4) . . ? C19 C14 C13 121.6(4) . . ? C14 C15 C16 120.9(5) . . ? C17 C16 C15 121.0(6) . . ? C16 C17 C18 118.9(5) . . ? C19 C18 C17 119.6(5) . . ? C18 C19 C14 121.2(5) . . ? N2 C20 C21 110.2(4) . . ? N3 C21 C20 109.6(4) . . ? N3 C22 C23 111.9(4) . . ? N4 C23 C24 121.5(5) . . ? N4 C23 C22 116.1(4) . . ? C24 C23 C22 122.4(5) . . ? C25 C24 C23 119.4(6) . . ? C24 C25 C26 119.3(5) . . ? C27 C26 C25 118.6(6) . . ? N4 C27 C26 122.5(5) . . ? N3 C28 C29 110.0(4) . . ? N5 C29 C30 122.6(6) . . ? N5 C29 C28 114.2(4) . . ? C30 C29 C28 123.1(6) . . ? C29 C30 C31 117.6(6) . . ? C32 C31 C30 120.4(6) . . ? C31 C32 C33 119.9(6) . . ? N5 C33 C32 121.0(6) . . ? O3 C34 O4 127.0(6) . . ? O3 C34 C35 115.3(5) . . ? O4 C34 C35 117.5(5) . . ? F1 P1 F4 91.8(5) . . ? F1 P1 F2 91.8(4) . . ? F4 P1 F2 176.4(4) . . ? F1 P1 F3 179.7(4) . . ? F4 P1 F3 88.6(4) . . ? F2 P1 F3 87.8(4) . . ? F1 P1 F6 90.6(3) . . ? F4 P1 F6 87.5(2) . . ? F2 P1 F6 92.2(3) . . ? F3 P1 F6 89.5(2) . . ? F1 P1 F5 90.3(3) . . ? F4 P1 F5 91.0(2) . . ? F2 P1 F5 89.2(2) . . ? F3 P1 F5 89.5(2) . . ? F6 P1 F5 178.3(2) . . ? C50 C51 O5 127(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.267 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.098 #===END data_complex_10 _database_code_CSD 170797 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H63 F6 Mn2 N5 O8 P' _chemical_formula_weight 1032.83 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 12.1741(2) _cell_length_b 13.5908(2) _cell_length_c 16.5007(2) _cell_angle_alpha 79.2919(8) _cell_angle_beta 68.9785(3) _cell_angle_gamma 79.8058(8) _cell_volume 2485.88(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.8134 _exptl_absorpt_correction_T_max 0.9524 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 10430 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4417 _reflns_number_gt 4062 _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^)+(0.1000P)^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 4417 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.3224 _refine_ls_wR_factor_gt 0.3149 _refine_ls_goodness_of_fit_ref 2.723 _refine_ls_restrained_S_all 2.723 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.003 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 0.92910(12) 0.78379(11) 0.25743(9) 0.0257(7) Uani 1 1 d . . . Mn2 Mn 0.66009(12) 0.80461(10) 0.32147(9) 0.0256(7) Uani 1 1 d . . . P1 P 0.2817(4) 1.3830(3) 0.2903(3) 0.0422(13) Uani 1 1 d . . . O1 O 1.0424(7) 0.8691(5) 0.1821(5) 0.033(2) Uani 1 1 d . . . O2 O 0.8102(5) 0.6994(4) 0.3284(4) 0.024(2) Uani 1 1 d . . . O3 O 0.8080(6) 0.8520(5) 0.2129(4) 0.031(2) Uani 1 1 d . . . O4 O 0.8756(6) 0.8761(5) 0.3662(5) 0.039(2) Uani 1 1 d . . . O5 O 0.6752(6) 0.8912(5) 0.4103(4) 0.039(2) Uani 1 1 d . . . O6 O 0.9858(6) 0.6905(5) 0.1411(4) 0.042(2) Uani 1 1 d . . . O7 O 0.8850(9) 0.7600(8) 0.0176(6) 0.089(4) Uani 1 1 d . . . O8 O 1.0861(7) 0.8796(6) 0.3963(6) 0.072(3) Uani 1 1 d . . . N1 N 1.0572(8) 0.7002(6) 0.2988(5) 0.030(3) Uani 1 1 d . . . N2 N 0.5266(7) 0.7021(6) 0.4289(5) 0.030(3) Uani 1 1 d . . . N3 N 0.5885(7) 0.7305(5) 0.2366(5) 0.026(3) Uani 1 1 d . . . N4 N 0.5332(7) 0.9255(6) 0.2751(5) 0.032(3) Uani 1 1 d . . . N5 N 0.6088(9) 0.5080(8) 0.1561(8) 0.084(4) Uani 1 1 d . . . C1 C 1.1487(12) 0.8350(9) 0.1364(8) 0.035(2) Uiso 1 1 d . . . C2 C 1.2058(12) 0.8865(10) 0.0504(9) 0.060(3) Uiso 1 1 d . . . H2A H 1.1655 0.9444 0.0279 0.072 Uiso 1 1 calc R . . C3 C 1.3219(12) 0.8505(10) -0.0002(9) 0.059(3) Uiso 1 1 d . . . H3A H 1.3582 0.8849 -0.0561 0.071 Uiso 1 1 calc R . . C4 C 1.3823(12) 0.7661(9) 0.0310(8) 0.051(3) Uiso 1 1 d . . . H4A H 1.4588 0.7420 -0.0039 0.061 Uiso 1 1 calc R . . C5 C 1.3310(10) 0.7169(8) 0.1131(7) 0.039(2) Uiso 1 1 d . . . H5A H 1.3753 0.6612 0.1348 0.047 Uiso 1 1 calc R . . C6 C 1.2164(9) 0.7463(8) 0.1652(7) 0.0282(18) Uiso 1 1 d . . . C7 C 1.1684(9) 0.6919(7) 0.2515(7) 0.0286(18) Uiso 1 1 d . . . H7A H 1.2213 0.6476 0.2750 0.034 Uiso 1 1 calc R . . C8 C 1.0233(10) 0.6460(8) 0.3892(7) 0.044(2) Uiso 1 1 d . . . H8A H 0.9979 0.6952 0.4308 0.053 Uiso 1 1 calc R . . H8B H 1.0928 0.6025 0.3976 0.053 Uiso 1 1 calc R . . C9 C 0.9246(9) 0.5823(8) 0.4085(7) 0.042(2) Uiso 1 1 d . . . H9A H 0.9167 0.5383 0.4640 0.051 Uiso 1 1 calc R . . H9B H 0.9462 0.5392 0.3623 0.051 Uiso 1 1 calc R . . C10 C 0.8044(9) 0.6447(7) 0.4145(6) 0.0319(19) Uiso 1 1 d . . . H10A H 0.7897 0.6950 0.4548 0.038 Uiso 1 1 calc R . . C11 C 0.7020(9) 0.5812(8) 0.4506(7) 0.042(2) Uiso 1 1 d . . . H11A H 0.6991 0.5500 0.4025 0.051 Uiso 1 1 calc R . . H11B H 0.7192 0.5266 0.4939 0.051 Uiso 1 1 calc R . . C12 C 0.5799(10) 0.6358(8) 0.4932(7) 0.043(2) Uiso 1 1 d . . . H12A H 0.5264 0.5857 0.5277 0.052 Uiso 1 1 calc R . . H12B H 0.5855 0.6777 0.5336 0.052 Uiso 1 1 calc R . . C13 C 0.4280(9) 0.7774(8) 0.4745(7) 0.036(2) Uiso 1 1 d . . . H13A H 0.4611 0.8182 0.5012 0.043 Uiso 1 1 calc R . . H13B H 0.4014 0.8228 0.4298 0.043 Uiso 1 1 calc R . . C14 C 0.3227(10) 0.7385(8) 0.5429(7) 0.041(2) Uiso 1 1 d . . . C15 C 0.3207(12) 0.7053(9) 0.6296(9) 0.066(3) Uiso 1 1 d . . . H15A H 0.3887 0.7054 0.6441 0.079 Uiso 1 1 calc R . . C16 C 0.2176(14) 0.6723(12) 0.6947(11) 0.088(4) Uiso 1 1 d . . . H16A H 0.2154 0.6537 0.7530 0.106 Uiso 1 1 calc R . . C17 C 0.1231(13) 0.6674(10) 0.6732(9) 0.072(3) Uiso 1 1 d . . . H17A H 0.0559 0.6422 0.7163 0.086 Uiso 1 1 calc R . . C18 C 0.1217(12) 0.6984(9) 0.5896(8) 0.063(3) Uiso 1 1 d . . . H18A H 0.0538 0.6955 0.5760 0.075 Uiso 1 1 calc R . . C19 C 0.2209(10) 0.7338(8) 0.5255(8) 0.049(2) Uiso 1 1 d . . . H19A H 0.2191 0.7554 0.4684 0.058 Uiso 1 1 calc R . . C20 C 0.4854(9) 0.6383(7) 0.3840(6) 0.036(2) Uiso 1 1 d . . . H20A H 0.4074 0.6195 0.4221 0.043 Uiso 1 1 calc R . . H20B H 0.5404 0.5762 0.3746 0.043 Uiso 1 1 calc R . . C21 C 0.4764(8) 0.6915(7) 0.2948(6) 0.0275(17) Uiso 1 1 d . . . H21A H 0.4566 0.6437 0.2659 0.033 Uiso 1 1 calc R . . H21B H 0.4123 0.7476 0.3047 0.033 Uiso 1 1 calc R . . C22 C 0.5705(9) 0.8089(7) 0.1669(7) 0.034(2) Uiso 1 1 d . . . H22A H 0.5207 0.7869 0.1401 0.041 Uiso 1 1 calc R . . H22B H 0.6471 0.8199 0.1215 0.041 Uiso 1 1 calc R . . C23 C 0.5106(9) 0.9084(8) 0.2046(7) 0.040(2) Uiso 1 1 d . . . C24 C 0.4421(11) 0.9807(9) 0.1648(8) 0.060(3) Uiso 1 1 d . . . H24A H 0.4204 0.9658 0.1196 0.072 Uiso 1 1 calc R . . C25 C 0.4076(14) 1.0726(12) 0.1927(10) 0.090(4) Uiso 1 1 d . . . H25A H 0.3701 1.1250 0.1624 0.108 Uiso 1 1 calc R . . C26 C 0.4283(12) 1.0885(11) 0.2666(9) 0.073(3) Uiso 1 1 d . . . H26A H 0.3984 1.1498 0.2898 0.088 Uiso 1 1 calc R . . C27 C 0.4921(11) 1.0148(9) 0.3052(8) 0.056(3) Uiso 1 1 d . . . H27A H 0.5077 1.0267 0.3541 0.067 Uiso 1 1 calc R . . C28 C 0.6833(9) 0.6476(7) 0.1993(6) 0.0336(19) Uiso 1 1 d . . . H28A H 0.6880 0.5947 0.2476 0.040 Uiso 1 1 calc R . . H28B H 0.7595 0.6751 0.1748 0.040 Uiso 1 1 calc R . . C29 C 0.6676(9) 0.5988(8) 0.1287(7) 0.035(2) Uiso 1 1 d . . . C30 C 0.7076(8) 0.6393(7) 0.0470(6) 0.0237(16) Uiso 1 1 d . . . H30A H 0.7925 0.6423 0.0327 0.028 Uiso 1 1 calc R . . H30B H 0.6697 0.7091 0.0440 0.028 Uiso 1 1 calc R . . C31 C 0.6963(10) 0.5993(8) -0.0169(8) 0.048(2) Uiso 1 1 d . . . H31A H 0.7246 0.6303 -0.0752 0.057 Uiso 1 1 calc R . . C32 C 0.6406(10) 0.5090(8) 0.0034(7) 0.045(2) Uiso 1 1 d . . . H32A H 0.6325 0.4803 -0.0414 0.053 Uiso 1 1 calc R . . C33 C 0.5988(10) 0.4642(9) 0.0899(8) 0.048(2) Uiso 1 1 d . . . H33A H 0.5636 0.4043 0.1036 0.058 Uiso 1 1 calc R . . C34 C 0.7727(12) 0.9093(8) 0.4136(8) 0.036(2) Uiso 1 1 d . . . C35 C 0.7644(11) 0.9726(9) 0.4808(8) 0.065(3) Uiso 1 1 d . . . H35A H 0.8435 0.9816 0.4770 0.097 Uiso 1 1 calc R . . H35B H 0.7236 0.9395 0.5387 0.097 Uiso 1 1 calc R . . H35C H 0.7207 1.0379 0.4705 0.097 Uiso 1 1 calc R . . C36 C 0.8214(11) 0.9442(9) 0.1523(8) 0.050(3) Uiso 1 1 d . . . H36A H 0.7614 0.9543 0.1238 0.060 Uiso 1 1 calc R . . H36B H 0.8996 0.9380 0.1067 0.060 Uiso 1 1 calc R . . C37 C 0.8085(12) 1.0364(9) 0.1979(8) 0.062(3) Uiso 1 1 d . . . H37A H 0.8195 1.0963 0.1549 0.094 Uiso 1 1 calc R . . H37B H 0.8678 1.0268 0.2262 0.094 Uiso 1 1 calc R . . H37C H 0.7301 1.0443 0.2416 0.094 Uiso 1 1 calc R . . C38 C 1.0449(14) 0.5944(11) 0.1262(11) 0.088(4) Uiso 1 1 d . . . H38A H 1.1160 0.6029 0.0744 0.105 Uiso 1 1 calc R . . H38B H 1.0722 0.5668 0.1759 0.105 Uiso 1 1 calc R . . C39 C 0.9892(15) 0.5216(11) 0.1138(11) 0.094(4) Uiso 1 1 d . . . H39A H 1.0451 0.4615 0.1005 0.142 Uiso 1 1 calc R . . H39B H 0.9598 0.5466 0.0654 0.142 Uiso 1 1 calc R . . H39C H 0.9234 0.5053 0.1666 0.142 Uiso 1 1 calc R . . C40 C 1.1487(11) 0.9572(9) 0.3410(8) 0.057(3) Uiso 1 1 d . . . H40A H 1.1704 0.9449 0.2802 0.069 Uiso 1 1 calc R . . H40B H 1.2223 0.9550 0.3531 0.069 Uiso 1 1 calc R . . C41 C 1.0835(13) 1.0589(10) 0.3497(10) 0.084(4) Uiso 1 1 d . . . H41A H 1.1327 1.1083 0.3095 0.125 Uiso 1 1 calc R . . H41B H 1.0632 1.0728 0.4092 0.125 Uiso 1 1 calc R . . H41C H 1.0115 1.0627 0.3361 0.125 Uiso 1 1 calc R . . C42 C 0.9375(19) 0.8041(17) -0.0607(15) 0.130(7) Uiso 1 1 d . . . H42A H 1.0087 0.7584 -0.0863 0.156 Uiso 1 1 calc R . . H42B H 0.9652 0.8639 -0.0527 0.156 Uiso 1 1 calc R . . C43 C 0.885(2) 0.8360(19) -0.1255(16) 0.177(9) Uiso 1 1 d . . . H43A H 0.9436 0.8627 -0.1792 0.265 Uiso 1 1 calc R . . H43B H 0.8198 0.8882 -0.1062 0.265 Uiso 1 1 calc R . . H43C H 0.8561 0.7793 -0.1361 0.265 Uiso 1 1 calc R . . F1 F 0.2730(14) 1.2993(7) 0.3684(7) 0.156(6) Uani 1 1 d . . . F2 F 0.3108(12) 1.4609(7) 0.3371(7) 0.147(5) Uani 1 1 d . . . F3 F 0.3078(12) 1.4664(8) 0.2099(7) 0.135(5) Uani 1 1 d . . . F4 F 0.2589(14) 1.3086(7) 0.2415(8) 0.182(6) Uani 1 1 d . . . F5 F 0.1563(11) 1.4268(9) 0.3158(13) 0.226(9) Uani 1 1 d . . . F6 F 0.4105(10) 1.3449(8) 0.2665(11) 0.192(7) 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 0.0245(13) 0.0279(12) 0.0234(12) 0.0013(9) -0.0088(10) -0.0033(10) Mn2 0.0246(12) 0.0244(12) 0.0266(12) 0.0001(9) -0.0085(10) -0.0037(9) P1 0.047(3) 0.031(3) 0.042(3) -0.008(3) -0.016(2) 0.017(2) O1 0.025(6) 0.025(5) 0.045(6) 0.002(4) -0.010(5) 0.000(4) O2 0.025(5) 0.021(4) 0.020(5) 0.007(4) -0.010(4) 0.004(4) O3 0.026(5) 0.027(5) 0.037(5) 0.001(4) -0.010(4) 0.002(4) O4 0.024(6) 0.054(5) 0.038(5) -0.024(4) -0.003(5) -0.002(4) O5 0.041(5) 0.032(4) 0.049(5) -0.005(4) -0.025(5) 0.000(4) O6 0.032(5) 0.041(5) 0.051(5) -0.027(4) -0.010(5) 0.008(4) O7 0.105(8) 0.142(9) 0.031(6) 0.031(6) -0.028(6) -0.075(8) O8 0.078(7) 0.063(6) 0.089(8) 0.011(6) -0.045(6) -0.029(6) N1 0.043(7) 0.038(6) 0.008(5) 0.013(5) -0.007(5) -0.021(5) N2 0.024(6) 0.026(6) 0.038(6) -0.003(5) -0.015(5) 0.013(5) N3 0.032(6) 0.019(5) 0.028(5) 0.006(5) -0.020(5) 0.004(5) N4 0.022(6) 0.032(6) 0.032(6) 0.002(5) -0.001(5) 0.001(5) N5 0.072(8) 0.096(9) 0.104(10) -0.046(8) -0.034(8) -0.016(7) F1 0.336(19) 0.055(7) 0.066(7) 0.028(6) -0.063(10) -0.049(9) F2 0.278(14) 0.080(7) 0.144(9) -0.008(6) -0.145(10) -0.023(8) F3 0.232(14) 0.085(8) 0.068(8) 0.011(7) -0.042(9) -0.008(9) F4 0.354(18) 0.087(7) 0.195(11) -0.049(7) -0.200(13) 0.006(9) F5 0.055(9) 0.093(9) 0.44(3) -0.028(12) 0.006(12) 0.022(8) F6 0.052(9) 0.062(8) 0.36(2) 0.044(11) 0.006(11) 0.027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.896(7) . ? Mn1 O3 1.901(6) . ? Mn1 O2 1.912(6) . ? Mn1 N1 2.010(8) . ? Mn1 O4 2.220(6) . ? Mn1 O6 2.326(6) . ? Mn1 Mn2 3.0367(19) . ? Mn2 O5 2.117(5) . ? Mn2 O3 2.130(7) . ? Mn2 O2 2.136(6) . ? Mn2 N4 2.270(9) . ? Mn2 N3 2.333(5) . ? Mn2 N2 2.354(9) . ? P1 F5 1.474(12) . ? P1 F6 1.492(11) . ? P1 F4 1.520(7) . ? P1 F1 1.537(10) . ? P1 F3 1.554(11) . ? P1 F2 1.572(8) . ? O1 C1 1.294(13) . ? O2 C10 1.460(11) . ? O3 C36 1.445(13) . ? O4 C34 1.269(13) . ? O5 C34 1.275(12) . ? O6 C38 1.395(15) . ? O7 C42 1.30(2) . ? O8 C40 1.397(13) . ? N1 C7 1.294(12) . ? N1 C8 1.481(13) . ? N2 C20 1.488(9) . ? N2 C13 1.502(12) . ? N2 C12 1.513(12) . ? N3 C22 1.465(11) . ? N3 C21 1.480(11) . ? N3 C28 1.507(12) . ? N4 C27 1.342(14) . ? N4 C23 1.354(11) . ? N5 C33 1.387(12) . ? N5 C29 1.453(14) . ? C1 C6 1.441(14) . ? C1 C2 1.443(15) . ? C2 C3 1.413(16) . ? C3 C4 1.369(15) . ? C4 C5 1.370(14) . ? C5 C6 1.384(13) . ? C6 C7 1.442(14) . ? C8 C9 1.512(12) . ? C9 C10 1.535(14) . ? C10 C11 1.520(13) . ? C11 C12 1.519(14) . ? C13 C14 1.475(14) . ? C14 C19 1.383(13) . ? C14 C15 1.411(16) . ? C15 C16 1.408(18) . ? C16 C17 1.336(17) . ? C17 C18 1.370(17) . ? C18 C19 1.382(16) . ? C20 C21 1.547(13) . ? C22 C23 1.545(13) . ? C23 C24 1.397(15) . ? C24 C25 1.356(18) . ? C25 C26 1.391(17) . ? C26 C27 1.362(16) . ? C28 C29 1.524(10) . ? C29 C30 1.306(12) . ? C30 C31 1.331(10) . ? C31 C32 1.434(13) . ? C32 C33 1.390(14) . ? C34 C35 1.492(13) . ? C36 C37 1.536(14) . ? C38 C39 1.376(17) . ? C40 C41 1.471(16) . ? C42 C43 1.40(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O3 93.2(3) . . ? O1 Mn1 O2 176.6(2) . . ? O3 Mn1 O2 83.8(3) . . ? O1 Mn1 N1 88.8(3) . . ? O3 Mn1 N1 174.4(2) . . ? O2 Mn1 N1 94.1(3) . . ? O1 Mn1 O4 93.1(3) . . ? O3 Mn1 O4 93.7(3) . . ? O2 Mn1 O4 88.6(2) . . ? N1 Mn1 O4 91.4(3) . . ? O1 Mn1 O6 85.8(3) . . ? O3 Mn1 O6 85.6(3) . . ? O2 Mn1 O6 92.4(2) . . ? N1 Mn1 O6 89.3(3) . . ? O4 Mn1 O6 178.7(3) . . ? O1 Mn1 Mn2 133.5(2) . . ? O3 Mn1 Mn2 44.0(2) . . ? O2 Mn1 Mn2 44.27(19) . . ? N1 Mn1 Mn2 135.7(2) . . ? O4 Mn1 Mn2 76.17(17) . . ? O6 Mn1 Mn2 104.01(16) . . ? O5 Mn2 O3 96.8(2) . . ? O5 Mn2 O2 93.0(2) . . ? O3 Mn2 O2 73.3(3) . . ? O5 Mn2 N4 93.9(2) . . ? O3 Mn2 N4 91.7(3) . . ? O2 Mn2 N4 164.1(3) . . ? O5 Mn2 N3 163.8(3) . . ? O3 Mn2 N3 93.5(2) . . ? O2 Mn2 N3 101.8(2) . . ? N4 Mn2 N3 73.4(2) . . ? O5 Mn2 N2 95.2(3) . . ? O3 Mn2 N2 161.9(3) . . ? O2 Mn2 N2 92.5(3) . . ? N4 Mn2 N2 101.0(3) . . ? N3 Mn2 N2 78.1(2) . . ? O5 Mn2 Mn1 83.41(19) . . ? O3 Mn2 Mn1 38.35(18) . . ? O2 Mn2 Mn1 38.66(17) . . ? N4 Mn2 Mn1 128.4(2) . . ? N3 Mn2 Mn1 112.2(2) . . ? N2 Mn2 Mn1 130.6(2) . . ? F5 P1 F6 176.1(8) . . ? F5 P1 F4 91.0(8) . . ? F6 P1 F4 92.8(8) . . ? F5 P1 F1 98.8(9) . . ? F6 P1 F1 82.3(8) . . ? F4 P1 F1 88.8(5) . . ? F5 P1 F3 88.1(8) . . ? F6 P1 F3 90.7(8) . . ? F4 P1 F3 93.8(6) . . ? F1 P1 F3 172.6(8) . . ? F5 P1 F2 91.0(8) . . ? F6 P1 F2 85.2(8) . . ? F4 P1 F2 177.3(8) . . ? F1 P1 F2 92.7(5) . . ? F3 P1 F2 84.4(5) . . ? C1 O1 Mn1 122.9(7) . . ? C10 O2 Mn1 124.8(4) . . ? C10 O2 Mn2 116.9(6) . . ? Mn1 O2 Mn2 97.1(3) . . ? C36 O3 Mn1 123.1(6) . . ? C36 O3 Mn2 131.1(7) . . ? Mn1 O3 Mn2 97.6(3) . . ? C34 O4 Mn1 129.7(4) . . ? C34 O5 Mn2 125.0(7) . . ? C38 O6 Mn1 134.5(8) . . ? C7 N1 C8 117.7(9) . . ? C7 N1 Mn1 123.8(7) . . ? C8 N1 Mn1 118.4(7) . . ? C20 N2 C13 111.7(7) . . ? C20 N2 C12 109.8(7) . . ? C13 N2 C12 110.6(8) . . ? C20 N2 Mn2 108.3(6) . . ? C13 N2 Mn2 103.1(6) . . ? C12 N2 Mn2 113.2(6) . . ? C22 N3 C21 112.1(7) . . ? C22 N3 C28 111.0(7) . . ? C21 N3 C28 112.3(7) . . ? C22 N3 Mn2 107.2(4) . . ? C21 N3 Mn2 107.7(4) . . ? C28 N3 Mn2 106.2(4) . . ? C27 N4 C23 119.1(10) . . ? C27 N4 Mn2 125.1(7) . . ? C23 N4 Mn2 115.3(7) . . ? C33 N5 C29 116.2(11) . . ? O1 C1 C6 124.2(11) . . ? O1 C1 C2 119.7(12) . . ? C6 C1 C2 116.1(13) . . ? C3 C2 C1 120.4(13) . . ? C4 C3 C2 120.8(14) . . ? C3 C4 C5 119.9(13) . . ? C4 C5 C6 122.3(12) . . ? C5 C6 C1 120.4(11) . . ? C5 C6 C7 119.5(10) . . ? C1 C6 C7 120.0(11) . . ? N1 C7 C6 124.3(10) . . ? N1 C8 C9 112.4(7) . . ? C8 C9 C10 113.5(8) . . ? O2 C10 C11 110.9(7) . . ? O2 C10 C9 109.3(8) . . ? C11 C10 C9 112.9(8) . . ? C12 C11 C10 116.5(8) . . ? N2 C12 C11 114.1(9) . . ? C14 C13 N2 117.8(8) . . ? C19 C14 C15 116.8(11) . . ? C19 C14 C13 121.8(9) . . ? C15 C14 C13 121.4(9) . . ? C16 C15 C14 120.5(11) . . ? C17 C16 C15 119.7(14) . . ? C16 C17 C18 121.5(15) . . ? C17 C18 C19 119.5(12) . . ? C18 C19 C14 121.9(11) . . ? N2 C20 C21 113.1(7) . . ? N3 C21 C20 111.9(7) . . ? N3 C22 C23 110.2(8) . . ? N4 C23 C24 121.2(9) . . ? N4 C23 C22 116.9(9) . . ? C24 C23 C22 121.7(8) . . ? C25 C24 C23 118.7(11) . . ? C24 C25 C26 119.4(15) . . ? C27 C26 C25 119.6(13) . . ? N4 C27 C26 121.6(10) . . ? N3 C28 C29 116.6(7) . . ? C30 C29 N5 123.0(7) . . ? C30 C29 C28 119.2(8) . . ? N5 C29 C28 117.8(10) . . ? C29 C30 C31 121.5(8) . . ? C30 C31 C32 119.7(11) . . ? C33 C32 C31 119.6(9) . . ? N5 C33 C32 120.0(10) . . ? O4 C34 O5 125.7(8) . . ? O4 C34 C35 117.5(8) . . ? O5 C34 C35 116.8(12) . . ? O3 C36 C37 112.1(9) . . ? C39 C38 O6 121.0(13) . . ? O8 C40 C41 114.5(11) . . ? O7 C42 C43 125.0(19) . . ? _diffrn_measured_fraction_theta_max 0.406 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.406 _refine_diff_density_max 0.869 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.099 #===END