# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Avarvari, Narcis' _publ_contact_author_email narcis.avarvari@univ-angers.fr _publ_author_name N.Avarvari # Attachment '- avarvari_revised.cif' #C3 Symmetric Tris(phosphonate)-1,3,5-triazine Ligand: #Homopolymetallic Complexes and Its Radical Anion data_L _database_code_depnum_ccdc_archive 'CCDC 765555' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H18 N3 O9 P3' _chemical_formula_weight 405.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.6958(8) _cell_length_b 11.0822(6) _cell_length_c 15.5505(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.187(7) _cell_angle_gamma 90.00 _cell_volume 1760.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 190 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13213 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4004 _reflns_number_gt 2735 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0489P)^2^+1.7584P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4004 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 C1A C 0.5795(2) 0.2465(2) 0.21261(18) 0.0269(6) Uani 1 1 d . . . C1B C 0.6386(5) 0.5937(5) 0.0673(4) 0.0877(17) Uani 1 1 d . . . H1B1 H 0.7249 0.6182 0.1017 0.132 Uiso 1 1 calc R A 1 H1B2 H 0.6099 0.6422 0.0139 0.132 Uiso 1 1 calc R A 1 H1B3 H 0.6399 0.5104 0.0508 0.132 Uiso 1 1 calc R A 1 C2B C 0.3524(4) 0.5756(4) 0.2156(4) 0.0792(15) Uani 1 1 d . . . H2B1 H 0.3098 0.5621 0.2610 0.119 Uiso 1 1 calc R B 1 H2B2 H 0.3624 0.5001 0.1880 0.119 Uiso 1 1 calc R B 1 H2B3 H 0.3005 0.6294 0.1707 0.119 Uiso 1 1 calc R B 1 C1 C 0.5127(4) -0.0482(3) 0.2483(3) 0.0559(10) Uani 1 1 d . . . H1A H 0.5563 -0.1249 0.2554 0.084 Uiso 1 1 calc R . . H1B H 0.4214 -0.0603 0.2414 0.084 Uiso 1 1 calc R . . H1C H 0.5505 0.0007 0.3005 0.084 Uiso 1 1 calc R . . C2A C 0.7553(3) 0.2909(2) 0.32880(18) 0.0270(6) Uani 1 1 d . . . C2 C 0.6021(4) 0.1504(4) 0.0263(3) 0.0607(10) Uani 1 1 d . . . H2A H 0.5891 0.1653 -0.0365 0.091 Uiso 1 1 calc R . . H2B H 0.6387 0.0713 0.0415 0.091 Uiso 1 1 calc R . . H2C H 0.6610 0.2096 0.0614 0.091 Uiso 1 1 calc R . . C3 C 1.0545(4) 0.3330(4) 0.5565(3) 0.0647(11) Uani 1 1 d . . . H3A H 1.0728 0.4104 0.5852 0.097 Uiso 1 1 calc R . . H3B H 1.1301 0.3049 0.5412 0.097 Uiso 1 1 calc R . . H3C H 1.0330 0.2766 0.5968 0.097 Uiso 1 1 calc R . . C4 C 0.8137(5) 0.0270(4) 0.4694(4) 0.0934(17) Uani 1 1 d . . . H4A H 0.7754 -0.0004 0.5145 0.140 Uiso 1 1 calc R . . H4B H 0.8961 -0.0128 0.4774 0.140 Uiso 1 1 calc R . . H4C H 0.7560 0.0085 0.4107 0.140 Uiso 1 1 calc R . . N1 N 0.6799(2) 0.2052(2) 0.27911(16) 0.0299(5) Uani 1 1 d . . . N3 N 0.7379(2) 0.4094(2) 0.31718(16) 0.0291(5) Uani 1 1 d . . . C3A C 0.6350(3) 0.4395(2) 0.24700(19) 0.0279(6) Uani 1 1 d . C . N2 N 0.5530(2) 0.3627(2) 0.19272(16) 0.0288(5) Uani 1 1 d . . . O1A O 0.4771(3) 0.6274(3) 0.2553(3) 0.0546(10) Uani 0.830(6) 1 d P C 1 O1B O 0.4570(11) 0.6130(11) 0.1720(12) 0.047(5) Uani 0.170(6) 1 d P C 2 O2 O 0.5277(2) 0.01202(18) 0.16920(16) 0.0413(5) Uani 1 1 d . . . O3 O 0.9452(2) 0.3435(2) 0.47548(17) 0.0576(7) Uani 1 1 d . . . O4 O 0.3324(2) 0.1558(2) 0.14553(17) 0.0465(6) Uani 1 1 d . . . O5 O 0.4778(2) 0.1578(2) 0.04534(15) 0.0455(6) Uani 1 1 d . . . O6 O 0.9852(2) 0.1685(2) 0.37872(16) 0.0528(7) Uani 1 1 d . . . O7 O 0.8337(2) 0.1537(3) 0.47749(17) 0.0593(7) Uani 1 1 d . . . O8A O 0.7115(5) 0.6752(5) 0.2704(4) 0.0598(15) Uani 0.830(6) 1 d P C 1 O8B O 0.665(3) 0.677(2) 0.298(2) 0.070(8) Uani 0.170(6) 1 d P C 2 O9A O 0.5498(3) 0.6094(3) 0.1206(2) 0.0492(10) Uani 0.830(6) 1 d P C 1 O9B O 0.6684(14) 0.6302(14) 0.1436(14) 0.061(6) Uani 0.170(6) 1 d P C 2 P1 P 0.46572(7) 0.13877(7) 0.14159(5) 0.0312(2) Uani 1 1 d . . . P2 P 0.89544(7) 0.23096(7) 0.41618(5) 0.0319(2) Uani 1 1 d . . . P3 P 0.60200(8) 0.60001(7) 0.22455(6) 0.0377(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 C1A 0.0295(13) 0.0237(13) 0.0280(14) -0.0009(12) 0.0093(11) 0.0000(11) C1B 0.097(4) 0.098(4) 0.082(4) 0.043(3) 0.048(3) 0.042(3) C2B 0.051(2) 0.057(3) 0.142(5) 0.003(3) 0.048(3) 0.006(2) C1 0.058(2) 0.042(2) 0.067(3) 0.0187(19) 0.0164(19) 0.0011(16) C2A 0.0290(13) 0.0263(14) 0.0266(14) 0.0010(11) 0.0096(11) 0.0021(11) C2 0.070(3) 0.069(3) 0.052(2) -0.014(2) 0.031(2) -0.018(2) C3 0.062(2) 0.070(3) 0.043(2) -0.010(2) -0.0131(18) -0.002(2) C4 0.090(3) 0.070(3) 0.113(5) 0.043(3) 0.019(3) -0.013(3) N1 0.0302(11) 0.0252(12) 0.0311(13) 0.0005(10) 0.0042(10) 0.0016(9) N3 0.0308(12) 0.0244(12) 0.0308(13) -0.0005(10) 0.0069(10) -0.0013(9) C3A 0.0301(14) 0.0241(13) 0.0306(15) -0.0009(12) 0.0106(11) -0.0004(11) N2 0.0299(11) 0.0233(12) 0.0307(13) 0.0009(10) 0.0052(9) 0.0000(9) O1A 0.0511(18) 0.0367(17) 0.080(3) -0.0051(16) 0.0251(17) 0.0055(13) O1B 0.029(7) 0.023(6) 0.083(14) 0.018(7) 0.006(7) 0.008(5) O2 0.0462(12) 0.0248(11) 0.0511(14) -0.0012(10) 0.0116(10) 0.0016(9) O3 0.0572(15) 0.0478(15) 0.0480(15) -0.0123(12) -0.0152(11) 0.0098(12) O4 0.0302(11) 0.0455(14) 0.0598(15) -0.0008(12) 0.0072(10) -0.0016(9) O5 0.0523(13) 0.0475(14) 0.0336(12) -0.0050(11) 0.0079(10) -0.0089(11) O6 0.0429(13) 0.0661(17) 0.0482(15) 0.0031(13) 0.0118(11) 0.0210(12) O7 0.0613(16) 0.0657(18) 0.0508(16) 0.0221(13) 0.0167(12) 0.0003(13) O8A 0.050(3) 0.031(2) 0.085(4) 0.004(2) -0.001(2) -0.0111(19) O8B 0.09(2) 0.026(10) 0.071(18) -0.012(10) -0.015(13) 0.021(13) O9A 0.049(2) 0.0425(17) 0.0522(19) 0.0157(14) 0.0095(13) 0.0096(13) O9B 0.044(9) 0.053(10) 0.088(14) 0.030(10) 0.024(8) 0.001(7) P1 0.0296(4) 0.0254(4) 0.0351(4) -0.0035(3) 0.0041(3) -0.0027(3) P2 0.0320(4) 0.0317(4) 0.0284(4) 0.0029(3) 0.0033(3) 0.0034(3) P3 0.0364(4) 0.0213(4) 0.0494(5) 0.0036(4) 0.0034(3) 0.0003(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 C1A N1 1.333(3) . ? C1A N2 1.335(3) . ? C1A P1 1.825(3) . ? C1B O9B 1.20(2) . ? C1B O9A 1.443(5) . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C2B O1A 1.415(5) . ? C2B O1B 1.526(15) . ? C2B H2B1 0.9600 . ? C2B H2B2 0.9600 . ? C2B H2B3 0.9600 . ? C1 O2 1.449(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2A N3 1.330(3) . ? C2A N1 1.335(3) . ? C2A P2 1.825(3) . ? C2 O5 1.447(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O3 1.448(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 O7 1.421(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N3 C3A 1.343(4) . ? C3A N2 1.330(3) . ? C3A P3 1.827(3) . ? O1A P3 1.576(3) . ? O1B P3 1.532(12) . ? O2 P1 1.558(2) . ? O3 P2 1.549(2) . ? O4 P1 1.457(2) . ? O5 P1 1.554(2) . ? O6 P2 1.439(2) . ? O7 P2 1.565(3) . ? O8A P3 1.442(6) . ? O8B P3 1.42(3) . ? O9A P3 1.550(3) . ? O9B P3 1.651(18) . ? 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 N1 C1A N2 125.3(2) . . ? N1 C1A P1 119.0(2) . . ? N2 C1A P1 115.67(19) . . ? O9B C1B O9A 54.6(7) . . ? O9B C1B H1B1 54.9 . . ? O9A C1B H1B1 109.5 . . ? O9B C1B H1B2 126.1 . . ? O9A C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? O9B C1B H1B3 124.4 . . ? O9A C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? O1A C2B O1B 50.5(6) . . ? O1A C2B H2B1 109.5 . . ? O1B C2B H2B1 160.0 . . ? O1A C2B H2B2 109.5 . . ? O1B C2B H2B2 81.1 . . ? H2B1 C2B H2B2 109.5 . . ? O1A C2B H2B3 109.5 . . ? O1B C2B H2B3 81.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2A N1 126.0(2) . . ? N3 C2A P2 120.8(2) . . ? N1 C2A P2 113.24(19) . . ? O5 C2 H2A 109.5 . . ? O5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O7 C4 H4A 109.5 . . ? O7 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O7 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1A N1 C2A 114.5(2) . . ? C2A N3 C3A 113.8(2) . . ? N2 C3A N3 125.8(2) . . ? N2 C3A P3 116.6(2) . . ? N3 C3A P3 117.6(2) . . ? C3A N2 C1A 114.6(2) . . ? C2B O1A P3 124.3(3) . . ? C2B O1B P3 119.8(11) . . ? C1 O2 P1 120.3(2) . . ? C3 O3 P2 120.0(2) . . ? C2 O5 P1 122.2(2) . . ? C4 O7 P2 124.5(3) . . ? C1B O9A P3 119.7(3) . . ? C1B O9B P3 129.4(12) . . ? O4 P1 O5 112.58(14) . . ? O4 P1 O2 116.53(13) . . ? O5 P1 O2 103.75(13) . . ? O4 P1 C1A 112.05(13) . . ? O5 P1 C1A 105.30(12) . . ? O2 P1 C1A 105.64(12) . . ? O6 P2 O3 118.37(15) . . ? O6 P2 O7 115.82(16) . . ? O3 P2 O7 102.15(16) . . ? O6 P2 C2A 111.91(13) . . ? O3 P2 C2A 102.24(13) . . ? O7 P2 C2A 104.56(13) . . ? O8B P3 O8A 30.2(11) . . ? O8B P3 O9B 106.4(14) . . ? O8A P3 O9B 77.9(7) . . ? O8B P3 O1B 122.6(12) . . ? O8A P3 O1B 139.1(5) . . ? O9B P3 O1B 99.8(9) . . ? O8B P3 O9A 137.5(12) . . ? O8A P3 O9A 117.8(3) . . ? O9B P3 O9A 45.2(6) . . ? O1B P3 O9A 56.0(7) . . ? O8B P3 O1A 83.4(11) . . ? O8A P3 O1A 112.1(2) . . ? O9B P3 O1A 141.8(5) . . ? O1B P3 O1A 47.8(7) . . ? O9A P3 O1A 103.12(18) . . ? O8B P3 C3A 114.0(11) . . ? O8A P3 C3A 112.7(3) . . ? O9B P3 C3A 103.9(6) . . ? O1B P3 C3A 107.5(5) . . ? O9A P3 C3A 104.75(15) . . ? O1A P3 C3A 105.26(14) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.524 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.075 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 765556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H24 Cu3 F36 N3 O21 P3' _chemical_formula_weight 1838.14 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' Cu Cu 0.3201 1.2651 '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' 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' P P 0.1023 0.0942 '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 11.5334(11) _cell_length_b 12.8817(17) _cell_length_c 23.900(3) _cell_angle_alpha 76.767(14) _cell_angle_beta 77.375(12) _cell_angle_gamma 78.485(14) _cell_volume 3330.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1806 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6996 _exptl_absorpt_correction_T_max 0.7077 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Rotation, Phi. incr. = 1' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33009 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.1683 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.94 _reflns_number_total 12084 _reflns_number_gt 3663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12084 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1803 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 0.724 _refine_ls_restrained_S_all 0.724 _refine_ls_shift/su_max 0.033 _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 C1 C 0.4787(6) -0.1231(5) 0.2910(2) 0.0552(17) Uani 1 1 d . . . C1A C 0.9448(8) -0.4840(6) 0.2740(3) 0.072(2) Uani 1 1 d . . . C1C C 0.3513(11) 0.2315(15) 0.2644(4) 0.155(7) Uani 1 1 d . . . C2 C 0.5788(7) -0.1476(5) 0.2013(3) 0.0655(19) Uani 1 1 d . . . C2A C 0.9636(11) -0.4834(12) 0.3340(4) 0.110(3) Uani 1 1 d . . . C2B C 0.3312(7) -0.2780(9) 0.5366(3) 0.080(2) Uani 1 1 d . . . C2C C 0.3262(8) 0.1941(6) 0.2120(3) 0.068(2) Uani 1 1 d . . . C3 C 0.3750(6) -0.1242(5) 0.2206(3) 0.0597(18) Uani 1 1 d . . . C3A C 1.0445(7) -0.4998(7) 0.2307(4) 0.091(2) Uani 1 1 d . . . H3A H 1.1206 -0.5074 0.2397 0.110 Uiso 1 1 calc R . . C3B C 0.2976(8) -0.3516(7) 0.5129(4) 0.089(3) Uani 1 1 d . . . H3B H 0.3264 -0.4245 0.5244 0.106 Uiso 1 1 calc R . . C3C C 0.4230(7) 0.1719(6) 0.1695(3) 0.076(2) Uani 1 1 d . . . H3C H 0.4996 0.1644 0.1779 0.091 Uiso 1 1 calc R . . C4 C 0.6213(10) -0.3086(8) 0.3816(4) 0.144(4) Uani 1 1 d . . . H4A H 0.6168 -0.3799 0.4046 0.216 Uiso 1 1 calc R . . H4B H 0.6839 -0.2799 0.3909 0.216 Uiso 1 1 calc R . . H4C H 0.6386 -0.3120 0.3408 0.216 Uiso 1 1 calc R . . C4A C 1.0360(8) -0.5046(6) 0.1754(4) 0.078(2) Uani 1 1 d . . . C4B C 0.2230(7) -0.3221(7) 0.4726(3) 0.077(2) Uani 1 1 d . . . C4C C 0.4134(7) 0.1603(6) 0.1156(3) 0.072(2) Uani 1 1 d . . . C5 C 0.5856(10) 0.0164(8) 0.3928(4) 0.145(4) Uani 1 1 d . . . H5A H 0.6632 0.0389 0.3825 0.218 Uiso 1 1 calc R . . H5B H 0.5687 -0.0113 0.4341 0.218 Uiso 1 1 calc R . . H5C H 0.5253 0.0769 0.3826 0.218 Uiso 1 1 calc R . . C5A C 1.1482(9) -0.5120(11) 0.1285(5) 0.110(3) Uani 1 1 d . . . C5C C 0.5251(8) 0.1464(10) 0.0700(4) 0.093(3) Uani 1 1 d . . . C6 C 0.6791(9) -0.1910(9) 0.0541(4) 0.141(4) Uani 1 1 d . . . H6A H 0.6685 -0.1450 0.0173 0.212 Uiso 1 1 calc R . . H6B H 0.6077 -0.2226 0.0715 0.212 Uiso 1 1 calc R . . H6C H 0.7464 -0.2473 0.0481 0.212 Uiso 1 1 calc R . . C6A C 0.4161(8) -0.4453(8) 0.2726(4) 0.078(2) Uani 1 1 d . . . C6B C 0.1830(13) 0.2053(9) 0.5100(6) 0.125(4) Uani 1 1 d . . . C6C C -0.2055(9) 0.2190(12) 0.2168(4) 0.111(3) Uani 1 1 d . . . C7 C 0.2797(11) -0.1593(11) 0.0958(4) 0.194(6) Uani 1 1 d . . . H7A H 0.2927 -0.2210 0.0777 0.291 Uiso 1 1 calc R . . H7B H 0.3501 -0.1250 0.0844 0.291 Uiso 1 1 calc R . . H7C H 0.2121 -0.1093 0.0836 0.291 Uiso 1 1 calc R . . C7A C 0.5282(8) -0.4567(6) 0.2264(3) 0.073(2) Uani 1 1 d . . . C7B C 0.1595(8) 0.1193(8) 0.4791(4) 0.084(2) Uani 1 1 d . . . C7C C -0.0947(7) 0.2070(6) 0.1706(3) 0.074(2) Uani 1 1 d . . . C8 C 0.0966(8) -0.1439(8) 0.3014(3) 0.129(4) Uani 1 1 d . . . H8A H 0.0549 -0.1981 0.3281 0.194 Uiso 1 1 calc R . . H8B H 0.0398 -0.0805 0.2911 0.194 Uiso 1 1 calc R . . H8C H 0.1544 -0.1260 0.3196 0.194 Uiso 1 1 calc R . . C8A C 0.5174(7) -0.4709(6) 0.1729(4) 0.085(2) Uani 1 1 d . . . H8A1 H 0.4411 -0.4685 0.1652 0.102 Uiso 1 1 calc R . . C8B C 0.0840(8) 0.1527(7) 0.4392(4) 0.086(2) Uani 1 1 d . . . H8B1 H 0.0504 0.2251 0.4306 0.103 Uiso 1 1 calc R . . C8C C -0.1065(7) 0.2034(7) 0.1160(3) 0.104(3) Uani 1 1 d . . . H8C1 H -0.1833 0.2099 0.1080 0.125 Uiso 1 1 calc R . . C9A C 0.6157(10) -0.4885(7) 0.1303(3) 0.085(2) Uani 1 1 d . . . C9B C 0.0577(7) 0.0800(8) 0.4118(3) 0.075(2) Uani 1 1 d . . . C9C C -0.0101(9) 0.1906(8) 0.0724(3) 0.102(3) Uani 1 1 d . . . C10 C 0.8912(12) -0.1224(11) 0.1933(7) 0.239(8) Uani 1 1 d . . . H10A H 0.9249 -0.0590 0.1914 0.358 Uiso 1 1 calc R . . H10B H 0.9525 -0.1753 0.1772 0.358 Uiso 1 1 calc R . . H10C H 0.8603 -0.1514 0.2333 0.358 Uiso 1 1 calc R . . C10A C 0.5900(13) -0.4971(14) 0.0706(6) 0.150(6) Uani 1 1 d . . . C10B C -0.0205(10) 0.1191(11) 0.3660(4) 0.111(3) Uani 1 1 d . . . C10C C -0.0384(13) 0.179(3) 0.0168(5) 0.293(16) Uani 1 1 d . . . C12B C 0.1866(13) -0.4258(18) 0.4606(9) 0.189(8) Uani 1 1 d . . . C20B C 0.433(2) -0.3252(12) 0.5746(6) 0.199(10) Uani 1 1 d . . . CuA Cu 0.78163(8) -0.46651(9) 0.19777(4) 0.0843(3) Uani 1 1 d . . . CuB Cu 0.20937(8) -0.09789(7) 0.46743(3) 0.0655(3) Uani 1 1 d . . . CuC Cu 0.15884(8) 0.17060(8) 0.14553(3) 0.0744(3) Uani 1 1 d . . . F1A F 1.1505(5) -0.5879(6) 0.0995(3) 0.163(3) Uani 1 1 d . . . F1B F 0.4521(16) -0.4142(8) 0.5873(7) 0.308(8) Uani 1 1 d . . . F1C F 0.5280(5) 0.2310(5) 0.0269(2) 0.136(2) Uani 1 1 d . . . F2 F 1.2465(5) -0.5542(6) 0.1526(3) 0.163(2) Uani 1 1 d . . . F2C F 0.5257(4) 0.0661(5) 0.0435(2) 0.1240(18) Uani 1 1 d . . . F3A F 1.1652(6) -0.4284(6) 0.0947(3) 0.203(4) Uani 1 1 d . . . F3C F 0.6248(5) 0.1262(5) 0.0904(2) 0.141(2) Uani 1 1 d . . . F4A F 1.0680(7) -0.5167(8) 0.3443(3) 0.213(4) Uani 1 1 d . . . F4C F 0.2682(8) 0.2857(8) 0.2889(3) 0.209(4) Uani 1 1 d . . . F5A F 0.8903(8) -0.5278(8) 0.3741(3) 0.218(4) Uani 1 1 d . . . F5B F 0.1908(13) -0.3876(8) 0.3991(5) 0.240(5) Uani 1 1 d . . . F5C F 0.4470(7) 0.2233(14) 0.2699(4) 0.318(8) Uani 1 1 d . . . F6A F 0.9384(8) -0.3856(7) 0.3435(3) 0.209(4) Uani 1 1 d . . . F6B F 0.2678(10) -0.4902(9) 0.4468(8) 0.284(6) Uani 1 1 d . . . F7A F 0.4123(4) -0.5282(4) 0.3144(2) 0.1150(17) Uani 1 1 d . . . F7B F -0.1046(6) 0.0634(6) 0.3708(2) 0.161(3) Uani 1 1 d . . . F8A F 0.4099(5) -0.3619(4) 0.2957(3) 0.140(2) Uani 1 1 d . . . F8B F -0.0799(7) 0.2151(6) 0.3672(3) 0.204(3) Uani 1 1 d . . . F8C F -0.3067(5) 0.2494(7) 0.1966(2) 0.184(3) Uani 1 1 d . . . F9A F 0.3169(5) -0.4317(5) 0.2525(2) 0.139(2) Uani 1 1 d . . . F9B F 0.0384(5) 0.1185(6) 0.3147(2) 0.180(3) Uani 1 1 d . . . F9C F -0.2062(5) 0.2921(6) 0.2469(3) 0.157(2) Uani 1 1 d . . . F10A F 0.4931(8) -0.4938(12) 0.0658(3) 0.291(7) Uani 1 1 d . . . F10C F -0.2166(5) 0.1336(6) 0.2555(3) 0.168(3) Uani 1 1 d . . . F11C F 0.3240(10) 0.1438(6) 0.3099(3) 0.210(4) Uani 1 1 d . . . F12A F 0.6472(12) -0.5966(8) 0.0621(4) 0.263(6) Uani 1 1 d . . . F12B F 0.4852(12) -0.2707(9) 0.5812(6) 0.261(6) Uani 1 1 d . . . F13B F 0.1381(10) 0.3011(6) 0.4882(4) 0.247(5) Uani 1 1 d . . . F14B F 0.1418(7) 0.1878(6) 0.5645(3) 0.192(3) Uani 1 1 d . . . F15B F 0.2951(9) 0.2047(6) 0.5042(4) 0.209(4) Uani 1 1 d . . . F20A F 0.6550(9) -0.4522(9) 0.0289(3) 0.223(5) Uani 1 1 d . . . F20B F 0.0898(9) -0.4268(10) 0.4688(6) 0.303(8) Uani 1 1 d . . . F20C F 0.0339(10) 0.1203(15) -0.0103(6) 0.284(7) Uani 1 1 d . . . F21B F 0.3600(8) -0.3145(16) 0.6301(3) 0.317(9) Uani 1 1 d . . . F21C F -0.1378(7) 0.2046(13) 0.0067(3) 0.338(8) Uani 1 1 d . . . F23C F 0.0135(12) 0.2705(17) -0.0254(5) 0.303(7) Uani 1 1 d . . . N1 N 0.5839(5) -0.1401(4) 0.2556(2) 0.0597(14) Uani 1 1 d . . . N2 N 0.3715(5) -0.1122(4) 0.2752(2) 0.0578(14) Uani 1 1 d . . . N3 N 0.4761(5) -0.1415(5) 0.1820(2) 0.0679(16) Uani 1 1 d . . . O1 O 0.7707(4) -0.2890(4) 0.1678(2) 0.0939(17) Uani 1 1 d . . . O1A O 0.6210(5) -0.4558(5) 0.2437(2) 0.0948(18) Uani 1 1 d . . . O1B O 0.1783(5) -0.2277(5) 0.4508(2) 0.0824(15) Uani 1 1 d . . . O1C O 0.2188(5) 0.2004(4) 0.20944(18) 0.0830(15) Uani 1 1 d . . . O2 O 0.7009(5) -0.1297(5) 0.0917(2) 0.1115(19) Uani 1 1 d . . . O2A O 0.7251(5) -0.4913(5) 0.1321(2) 0.0983(18) Uani 1 1 d . . . O2B O 0.3066(4) -0.1770(4) 0.52490(18) 0.0773(14) Uani 1 1 d . . . O2C O 0.3178(5) 0.1612(4) 0.09785(18) 0.0845(16) Uani 1 1 d . . . O3 O 0.3637(4) -0.0767(4) 0.39653(17) 0.0821(15) Uani 1 1 d . . . O3A O 0.8388(5) -0.4723(4) 0.26923(19) 0.0881(16) Uani 1 1 d . . . O3B O 0.0917(4) -0.0196(5) 0.41941(18) 0.0776(14) Uani 1 1 d . . . O3C O 0.0983(5) 0.1752(5) 0.07605(18) 0.0919(17) Uani 1 1 d . . . O4 O 0.5116(6) -0.2421(5) 0.3940(2) 0.1094(19) Uani 1 1 d . . . O4A O 0.9423(5) -0.4993(4) 0.1557(2) 0.0856(16) Uani 1 1 d . . . O4B O 0.2118(5) 0.0271(4) 0.49732(19) 0.0797(15) Uani 1 1 d . . . O4C O -0.0014(5) 0.1988(4) 0.18968(18) 0.0854(16) Uani 1 1 d . . . O5 O 0.5850(5) -0.0647(5) 0.3623(2) 0.1089(19) Uani 1 1 d . . . O6 O 0.1819(5) -0.0059(4) 0.1793(2) 0.0952(16) Uani 1 1 d . . . O7 O 0.2570(5) -0.1918(5) 0.1554(2) 0.117(2) Uani 1 1 d . . . O8 O 0.1559(4) -0.1834(4) 0.2509(2) 0.0912(15) Uani 1 1 d . . . O9 O 0.7996(5) -0.0958(5) 0.1619(2) 0.1051(18) Uani 1 1 d . . . P4 P 0.23174(18) -0.11539(19) 0.19875(8) 0.0704(6) Uani 1 1 d . . . P5 P 0.72205(19) -0.1766(2) 0.15385(8) 0.0793(7) Uani 1 1 d . . . P6 P 0.47839(19) -0.12177(17) 0.36672(7) 0.0651(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.057(5) 0.060(4) 0.053(4) -0.015(3) -0.015(4) -0.009(3) C1A 0.059(6) 0.077(5) 0.089(6) -0.012(4) -0.032(5) -0.016(4) C1C 0.070(8) 0.321(18) 0.053(5) -0.056(8) -0.036(5) 0.073(10) C2 0.065(5) 0.081(5) 0.052(4) -0.017(3) -0.014(4) -0.008(4) C2A 0.101(9) 0.170(11) 0.086(7) -0.042(7) -0.037(6) -0.038(8) C2B 0.085(6) 0.084(7) 0.066(5) -0.006(5) -0.012(4) -0.014(5) C2C 0.059(6) 0.080(5) 0.064(5) 0.008(4) -0.022(4) -0.021(4) C3 0.066(5) 0.064(5) 0.053(4) -0.016(3) -0.021(3) -0.001(4) C3A 0.059(6) 0.121(7) 0.099(6) -0.018(5) -0.033(5) -0.011(5) C3B 0.111(8) 0.051(5) 0.089(6) 0.006(5) -0.021(5) 0.001(5) C3C 0.054(5) 0.099(6) 0.073(5) -0.013(4) -0.018(4) -0.009(4) C4 0.172(11) 0.114(8) 0.139(8) -0.045(7) -0.064(7) 0.059(8) C4A 0.058(6) 0.077(6) 0.091(6) -0.008(4) -0.013(5) -0.003(4) C4B 0.075(6) 0.079(7) 0.073(5) -0.023(5) 0.001(4) -0.010(5) C4C 0.060(6) 0.079(5) 0.076(5) -0.012(4) -0.016(4) -0.011(4) C5 0.183(12) 0.134(9) 0.162(9) -0.059(8) -0.060(8) -0.058(8) C5A 0.061(7) 0.130(10) 0.125(8) -0.028(8) -0.011(7) 0.014(7) C5C 0.066(7) 0.144(9) 0.076(6) -0.035(6) -0.014(5) -0.014(6) C6 0.155(10) 0.191(11) 0.094(6) -0.046(7) -0.048(6) -0.016(8) C6A 0.052(6) 0.097(7) 0.089(6) -0.020(6) -0.015(5) -0.017(5) C6B 0.137(11) 0.074(8) 0.144(10) 0.004(7) -0.016(9) -0.009(8) C6C 0.073(8) 0.171(12) 0.084(7) -0.024(7) -0.002(6) -0.023(7) C7 0.188(13) 0.322(18) 0.096(8) -0.091(10) -0.013(7) -0.051(11) C7A 0.067(6) 0.073(5) 0.083(5) -0.016(4) -0.021(5) -0.012(4) C7B 0.106(8) 0.073(7) 0.078(5) -0.032(5) -0.005(5) -0.016(6) C7C 0.053(6) 0.097(6) 0.061(5) -0.003(4) -0.012(4) -0.004(4) C8 0.092(7) 0.207(11) 0.093(6) -0.054(7) 0.024(5) -0.049(7) C8A 0.061(6) 0.100(6) 0.101(6) -0.025(5) -0.027(5) -0.010(4) C8B 0.094(7) 0.066(6) 0.085(6) -0.004(5) -0.015(5) 0.003(5) C8C 0.061(6) 0.171(9) 0.077(5) -0.019(5) -0.029(5) 0.000(5) C9A 0.087(7) 0.102(7) 0.080(5) -0.029(5) -0.033(5) -0.014(5) C9B 0.066(6) 0.083(7) 0.058(4) 0.003(5) 0.001(4) -0.006(5) C9C 0.075(7) 0.171(9) 0.066(5) -0.028(5) -0.022(5) -0.014(6) C10 0.160(13) 0.204(15) 0.42(2) -0.053(14) -0.199(15) -0.030(10) C10A 0.107(11) 0.250(16) 0.147(11) -0.135(11) 0.027(9) -0.097(11) C10B 0.067(7) 0.144(10) 0.097(7) 0.006(7) -0.027(6) 0.020(7) C10C 0.080(11) 0.72(5) 0.068(8) -0.12(2) -0.013(7) 0.021(19) C12B 0.083(9) 0.31(2) 0.245(16) -0.242(16) -0.016(9) 0.008(11) C20B 0.44(3) 0.081(10) 0.127(10) 0.072(8) -0.171(15) -0.135(15) CuA 0.0565(7) 0.1266(9) 0.0787(6) -0.0394(6) -0.0191(5) -0.0051(6) CuB 0.0759(6) 0.0621(6) 0.0564(5) -0.0108(4) -0.0150(4) -0.0036(5) CuC 0.0549(6) 0.1100(8) 0.0589(5) -0.0139(5) -0.0153(4) -0.0114(5) F1A 0.112(5) 0.210(7) 0.158(5) -0.083(5) 0.034(4) -0.017(4) F1B 0.471(19) 0.123(7) 0.397(16) -0.030(9) -0.340(15) 0.059(9) F1C 0.124(5) 0.148(5) 0.107(4) -0.009(4) 0.031(3) -0.033(4) F2 0.073(4) 0.207(7) 0.180(5) -0.028(5) -0.001(4) 0.005(4) F2C 0.089(4) 0.158(5) 0.127(4) -0.066(4) 0.001(3) -0.002(3) F3A 0.161(6) 0.138(6) 0.207(7) 0.058(5) 0.067(5) -0.003(5) F3C 0.057(4) 0.239(7) 0.142(4) -0.081(4) -0.019(3) -0.005(4) F4A 0.131(6) 0.369(12) 0.169(6) -0.125(6) -0.099(5) 0.052(7) F4C 0.207(8) 0.285(11) 0.175(6) -0.135(7) -0.097(6) 0.038(7) F5A 0.223(9) 0.375(14) 0.084(4) -0.008(5) -0.044(5) -0.136(8) F5B 0.353(16) 0.173(9) 0.258(10) -0.113(7) -0.061(9) -0.102(10) F5C 0.098(6) 0.79(2) 0.155(6) -0.238(11) 0.007(5) -0.133(10) F6A 0.302(11) 0.192(7) 0.186(7) -0.099(6) -0.123(7) -0.007(7) F6B 0.211(10) 0.186(9) 0.526(19) -0.232(13) -0.096(11) 0.025(7) F7A 0.118(4) 0.111(4) 0.098(3) 0.001(3) -0.003(3) -0.018(3) F7B 0.106(5) 0.232(8) 0.133(4) 0.037(4) -0.058(4) -0.043(5) F8A 0.116(4) 0.109(4) 0.197(5) -0.084(4) 0.038(4) -0.035(3) F8B 0.220(8) 0.143(6) 0.248(8) -0.025(5) -0.144(6) 0.068(6) F8C 0.057(4) 0.353(10) 0.129(4) -0.056(5) -0.013(3) 0.004(5) F9A 0.061(4) 0.216(7) 0.136(4) -0.033(4) -0.021(3) -0.012(4) F9B 0.111(5) 0.320(9) 0.070(3) 0.023(4) -0.022(3) -0.006(5) F9C 0.129(5) 0.200(7) 0.133(4) -0.071(5) 0.021(4) -0.008(4) F10A 0.115(6) 0.66(2) 0.179(7) -0.218(10) -0.035(5) -0.083(10) F10C 0.123(5) 0.179(6) 0.146(5) 0.014(5) 0.052(4) -0.032(4) F11C 0.389(14) 0.171(7) 0.106(5) -0.017(4) -0.125(6) -0.050(7) F12A 0.449(17) 0.190(8) 0.223(8) -0.116(8) -0.212(9) 0.030(9) F12B 0.337(15) 0.165(9) 0.341(15) 0.034(8) -0.255(13) -0.061(9) F13B 0.390(14) 0.076(5) 0.310(10) -0.038(6) -0.175(9) 0.004(6) F14B 0.272(9) 0.174(7) 0.164(6) -0.101(6) -0.012(6) -0.070(6) F15B 0.180(7) 0.168(7) 0.318(10) -0.121(7) 0.007(8) -0.089(6) F20A 0.219(9) 0.388(15) 0.112(5) -0.100(7) -0.012(5) -0.125(9) F20B 0.156(8) 0.328(12) 0.500(19) -0.289(13) 0.112(10) -0.158(9) F20C 0.203(11) 0.57(2) 0.145(8) -0.185(14) -0.005(8) -0.124(12) F21B 0.165(8) 0.59(3) 0.112(6) 0.029(8) -0.073(5) 0.068(11) F21C 0.090(6) 0.84(3) 0.128(5) -0.157(9) -0.044(4) -0.074(10) F23C 0.244(12) 0.53(2) 0.096(6) 0.031(9) -0.083(7) -0.028(13) N1 0.053(4) 0.073(4) 0.055(3) -0.016(3) -0.010(3) -0.009(3) N2 0.048(4) 0.075(4) 0.055(3) -0.019(3) -0.012(3) -0.010(3) N3 0.058(4) 0.093(4) 0.056(3) -0.023(3) -0.015(3) -0.004(3) O1 0.079(4) 0.098(4) 0.097(4) -0.029(3) -0.011(3) 0.010(3) O1A 0.065(4) 0.151(5) 0.082(3) -0.044(3) -0.018(3) -0.017(3) O1B 0.094(4) 0.071(4) 0.087(3) -0.018(3) -0.029(3) -0.007(3) O1C 0.069(4) 0.120(4) 0.063(3) -0.019(3) -0.011(3) -0.021(3) O2 0.102(5) 0.156(5) 0.069(3) -0.025(3) -0.018(3) 0.003(4) O2A 0.072(4) 0.149(5) 0.089(4) -0.055(3) -0.016(3) -0.014(4) O2B 0.096(4) 0.065(4) 0.072(3) -0.004(3) -0.032(3) -0.008(3) O2C 0.060(4) 0.130(5) 0.065(3) -0.023(3) -0.012(3) -0.012(3) O3 0.077(3) 0.109(4) 0.059(3) -0.027(3) 0.000(2) -0.013(3) O3A 0.064(4) 0.128(5) 0.081(3) -0.031(3) -0.021(3) -0.016(3) O3B 0.081(4) 0.078(4) 0.072(3) -0.015(3) -0.023(2) 0.002(3) O3C 0.063(4) 0.145(5) 0.064(3) -0.024(3) -0.016(3) 0.001(3) O4 0.149(6) 0.093(4) 0.076(3) -0.007(3) -0.035(3) 0.011(4) O4A 0.062(4) 0.109(4) 0.082(3) -0.028(3) -0.017(3) 0.010(3) O4B 0.102(4) 0.063(4) 0.072(3) -0.013(3) -0.026(3) 0.002(3) O4C 0.061(4) 0.130(5) 0.063(3) -0.018(3) -0.019(3) -0.004(3) O5 0.086(4) 0.172(6) 0.098(4) -0.073(4) -0.003(3) -0.047(4) O6 0.082(4) 0.084(4) 0.118(4) 0.002(3) -0.047(3) -0.002(3) O7 0.099(5) 0.179(6) 0.103(4) -0.077(4) -0.037(3) -0.015(4) O8 0.077(4) 0.109(4) 0.093(4) -0.016(3) -0.022(3) -0.022(3) O9 0.064(4) 0.130(5) 0.121(4) -0.022(4) -0.007(3) -0.028(4) P4 0.0577(14) 0.0992(17) 0.0621(11) -0.0244(12) -0.0218(10) -0.0080(12) P5 0.0556(15) 0.117(2) 0.0634(12) -0.0259(13) -0.0107(10) 0.0008(14) P6 0.0703(15) 0.0737(15) 0.0566(10) -0.0192(10) -0.0195(10) -0.0077(11) _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 C1 N1 1.330(7) . ? C1 N2 1.343(7) . ? C1 P6 1.812(6) . ? C1A O3A 1.230(8) . ? C1A C3A 1.385(10) . ? C1A C2A 1.498(11) . ? C1C F5C 1.120(10) . ? C1C F4C 1.194(9) . ? C1C F11C 1.409(16) . ? C1C C2C 1.541(13) . ? C2 N1 1.338(7) . ? C2 N3 1.345(8) . ? C2 P5 1.812(7) . ? C2A F5A 1.244(11) . ? C2A F4A 1.252(11) . ? C2A F6A 1.296(12) . ? C2B O2B 1.255(9) . ? C2B C3B 1.364(11) . ? C2B C20B 1.585(18) . ? C2C O1C 1.240(8) . ? C2C C3C 1.367(9) . ? C3 N3 1.335(7) . ? C3 N2 1.340(7) . ? C3 P4 1.814(7) . ? C3A C4A 1.362(10) . ? C3A H3A 0.9300 . ? C3B C4B 1.369(11) . ? C3B H3B 0.9300 . ? C3C C4C 1.361(9) . ? C3C H3C 0.9300 . ? C4 O4 1.393(9) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4A O4A 1.253(9) . ? C4A C5A 1.518(11) . ? C4B O1B 1.262(9) . ? C4B C12B 1.580(18) . ? C4C O2C 1.262(8) . ? C4C C5C 1.504(10) . ? C5 O5 1.405(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5A F3A 1.212(11) . ? C5A F1A 1.315(11) . ? C5A F2 1.345(10) . ? C5C F3C 1.303(9) . ? C5C F1C 1.318(10) . ? C5C F2C 1.327(9) . ? C6 O2 1.412(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C6A F7A 1.285(9) . ? C6A F9A 1.301(8) . ? C6A F8A 1.299(8) . ? C6A C7A 1.512(10) . ? C6B F15B 1.268(12) . ? C6B F14B 1.269(11) . ? C6B F13B 1.277(11) . ? C6B C7B 1.559(14) . ? C6C F10C 1.273(11) . ? C6C F9C 1.306(11) . ? C6C F8C 1.313(10) . ? C6C C7C 1.503(11) . ? C7 O7 1.371(10) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7A O1A 1.232(8) . ? C7A C8A 1.368(10) . ? C7B O4B 1.247(9) . ? C7B C8B 1.371(11) . ? C7C O4C 1.234(8) . ? C7C C8C 1.354(9) . ? C8 O8 1.402(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8A C9A 1.368(10) . ? C8A H8A1 0.9300 . ? C8B C9B 1.370(10) . ? C8B H8B1 0.9300 . ? C8C C9C 1.359(10) . ? C8C H8C1 0.9300 . ? C9A O2A 1.265(9) . ? C9A C10A 1.550(14) . ? C9B O3B 1.248(8) . ? C9B C10B 1.505(11) . ? C9C O3C 1.245(9) . ? C9C C10C 1.479(16) . ? C10 O9 1.372(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10A F10A 1.139(12) . ? C10A F20A 1.214(13) . ? C10A F12A 1.357(15) . ? C10B F9B 1.266(9) . ? C10B F7B 1.289(12) . ? C10B F8B 1.292(11) . ? C10C F20C 1.20(3) . ? C10C F21C 1.189(14) . ? C10C F23C 1.49(4) . ? C12B F20B 1.092(12) . ? C12B F6B 1.163(13) . ? C12B F5B 1.43(2) . ? C20B F12B 1.064(13) . ? C20B F1B 1.107(12) . ? C20B F21B 1.43(2) . ? CuA O4A 1.922(5) . ? CuA O1A 1.933(5) . ? CuA O2A 1.936(5) . ? CuA O3A 1.942(5) . ? CuA O1 2.221(6) . ? CuB O4B 1.913(5) . ? CuB O1B 1.920(5) . ? CuB O2B 1.939(5) . ? CuB O3B 1.944(5) . ? CuB O3 2.186(4) . ? CuC O3C 1.922(5) . ? CuC O4C 1.928(5) . ? CuC O2C 1.933(5) . ? CuC O1C 1.948(5) . ? CuC O6 2.214(5) . ? F5B F6B 1.767(15) . ? F12B F21B 1.748(15) . ? O1 P5 1.435(5) . ? O2 P5 1.524(5) . ? O3 P6 1.437(4) . ? O4 P6 1.544(6) . ? O5 P6 1.527(6) . ? O6 P4 1.425(5) . ? O7 P4 1.533(5) . ? O8 P4 1.555(5) . ? O9 P5 1.568(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 124.1(5) . . ? N1 C1 P6 118.5(5) . . ? N2 C1 P6 117.3(5) . . ? O3A C1A C3A 126.6(7) . . ? O3A C1A C2A 114.5(8) . . ? C3A C1A C2A 118.9(9) . . ? F5C C1C F4C 124.7(15) . . ? F5C C1C F11C 95.0(12) . . ? F4C C1C F11C 87.4(10) . . ? F5C C1C C2C 118.6(9) . . ? F4C C1C C2C 115.0(9) . . ? F11C C1C C2C 100.9(13) . . ? N1 C2 N3 124.2(6) . . ? N1 C2 P5 116.1(6) . . ? N3 C2 P5 119.6(5) . . ? F5A C2A F4A 109.6(12) . . ? F5A C2A F6A 100.5(10) . . ? F4A C2A F6A 104.8(10) . . ? F5A C2A C1A 113.8(10) . . ? F4A C2A C1A 116.6(9) . . ? F6A C2A C1A 109.9(10) . . ? O2B C2B C3B 128.3(8) . . ? O2B C2B C20B 115.6(9) . . ? C3B C2B C20B 115.0(9) . . ? O1C C2C C3C 126.5(7) . . ? O1C C2C C1C 116.0(7) . . ? C3C C2C C1C 116.8(8) . . ? N3 C3 N2 124.3(6) . . ? N3 C3 P4 118.8(5) . . ? N2 C3 P4 116.9(5) . . ? C4A C3A C1A 122.9(8) . . ? C4A C3A H3A 118.6 . . ? C1A C3A H3A 118.6 . . ? C2B C3B C4B 122.4(7) . . ? C2B C3B H3B 118.8 . . ? C4B C3B H3B 118.8 . . ? C4C C3C C2C 123.7(7) . . ? C4C C3C H3C 118.2 . . ? C2C C3C H3C 118.2 . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O4A C4A C3A 127.7(7) . . ? O4A C4A C5A 112.1(8) . . ? C3A C4A C5A 120.1(9) . . ? O1B C4B C3B 127.5(8) . . ? O1B C4B C12B 122.2(11) . . ? C3B C4B C12B 109.9(11) . . ? O2C C4C C3C 126.9(7) . . ? O2C C4C C5C 113.6(7) . . ? C3C C4C C5C 119.5(8) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? F3A C5A F1A 110.0(10) . . ? F3A C5A F2 109.3(11) . . ? F1A C5A F2 98.9(9) . . ? F3A C5A C4A 115.6(9) . . ? F1A C5A C4A 111.0(10) . . ? F2 C5A C4A 110.8(9) . . ? F3C C5C F1C 109.3(9) . . ? F3C C5C F2C 107.0(8) . . ? F1C C5C F2C 103.3(7) . . ? F3C C5C C4C 114.0(7) . . ? F1C C5C C4C 111.4(8) . . ? F2C C5C C4C 111.2(8) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? F7A C6A F9A 106.0(7) . . ? F7A C6A F8A 107.3(7) . . ? F9A C6A F8A 106.1(8) . . ? F7A C6A C7A 112.6(7) . . ? F9A C6A C7A 113.6(7) . . ? F8A C6A C7A 110.8(7) . . ? F15B C6B F14B 106.8(12) . . ? F15B C6B F13B 106.4(11) . . ? F14B C6B F13B 108.1(11) . . ? F15B C6B C7B 110.3(10) . . ? F14B C6B C7B 112.6(9) . . ? F13B C6B C7B 112.3(11) . . ? F10C C6C F9C 103.8(8) . . ? F10C C6C F8C 107.4(10) . . ? F9C C6C F8C 103.8(10) . . ? F10C C6C C7C 113.3(10) . . ? F9C C6C C7C 113.1(10) . . ? F8C C6C C7C 114.5(8) . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1A C7A C8A 128.0(7) . . ? O1A C7A C6A 113.3(7) . . ? C8A C7A C6A 118.6(8) . . ? O4B C7B C8B 130.1(8) . . ? O4B C7B C6B 112.0(9) . . ? C8B C7B C6B 117.9(9) . . ? O4C C7C C8C 128.4(7) . . ? O4C C7C C6C 112.4(7) . . ? C8C C7C C6C 119.2(9) . . ? O8 C8 H8A 109.5 . . ? O8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7A C8A C9A 121.8(8) . . ? C7A C8A H8A1 119.1 . . ? C9A C8A H8A1 119.1 . . ? C7B C8B C9B 120.3(8) . . ? C7B C8B H8B1 119.8 . . ? C9B C8B H8B1 119.8 . . ? C7C C8C C9C 122.3(8) . . ? C7C C8C H8C1 118.8 . . ? C9C C8C H8C1 118.8 . . ? O2A C9A C8A 127.9(7) . . ? O2A C9A C10A 115.5(9) . . ? C8A C9A C10A 116.4(9) . . ? O3B C9B C8B 128.0(8) . . ? O3B C9B C10B 112.4(9) . . ? C8B C9B C10B 119.5(9) . . ? O3C C9C C8C 127.4(7) . . ? O3C C9C C10C 116.8(9) . . ? C8C C9C C10C 115.3(10) . . ? O9 C10 H10A 109.5 . . ? O9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F10A C10A F20A 116.6(18) . . ? F10A C10A F12A 105.4(12) . . ? F20A C10A F12A 92.5(10) . . ? F10A C10A C9A 119.1(10) . . ? F20A C10A C9A 113.5(10) . . ? F12A C10A C9A 104.6(13) . . ? F9B C10B F7B 104.6(10) . . ? F9B C10B F8B 107.9(10) . . ? F7B C10B F8B 102.4(9) . . ? F9B C10B C9B 112.8(8) . . ? F7B C10B C9B 115.0(10) . . ? F8B C10B C9B 113.2(10) . . ? F20C C10C F21C 120(2) . . ? F20C C10C C9C 116.1(17) . . ? F21C C10C C9C 121.5(14) . . ? F20C C10C F23C 86.9(11) . . ? F21C C10C F23C 97(2) . . ? C9C C10C F23C 102(2) . . ? F20B C12B F6B 130.9(19) . . ? F20B C12B F5B 92.5(17) . . ? F6B C12B F5B 85.0(12) . . ? F20B C12B C4B 114.7(12) . . ? F6B C12B C4B 114.3(12) . . ? F5B C12B C4B 96.1(16) . . ? F12B C20B F1B 125(2) . . ? F12B C20B F21B 87.7(15) . . ? F1B C20B F21B 92.5(13) . . ? F12B C20B C2B 118.2(13) . . ? F1B C20B C2B 116.0(13) . . ? F21B C20B C2B 97.0(15) . . ? O4A CuA O1A 171.7(2) . . ? O4A CuA O2A 87.3(2) . . ? O1A CuA O2A 91.7(2) . . ? O4A CuA O3A 92.3(2) . . ? O1A CuA O3A 87.1(2) . . ? O2A CuA O3A 168.6(3) . . ? O4A CuA O1 94.6(2) . . ? O1A CuA O1 93.7(2) . . ? O2A CuA O1 95.9(2) . . ? O3A CuA O1 95.6(2) . . ? O4B CuB O1B 167.8(2) . . ? O4B CuB O2B 86.1(2) . . ? O1B CuB O2B 92.8(2) . . ? O4B CuB O3B 92.2(2) . . ? O1B CuB O3B 87.0(2) . . ? O2B CuB O3B 171.5(2) . . ? O4B CuB O3 96.33(19) . . ? O1B CuB O3 95.92(18) . . ? O2B CuB O3 94.20(19) . . ? O3B CuB O3 94.29(18) . . ? O3C CuC O4C 91.9(2) . . ? O3C CuC O2C 87.2(2) . . ? O4C CuC O2C 173.0(2) . . ? O3C CuC O1C 167.2(2) . . ? O4C CuC O1C 87.8(2) . . ? O2C CuC O1C 91.5(2) . . ? O3C CuC O6 99.3(2) . . ? O4C CuC O6 94.8(2) . . ? O2C CuC O6 92.2(2) . . ? O1C CuC O6 93.5(2) . . ? C12B F5B F6B 41.0(6) . . ? C12B F6B F5B 54.0(12) . . ? C20B F12B F21B 54.8(14) . . ? C20B F21B F12B 37.5(6) . . ? C1 N1 C2 116.0(6) . . ? C3 N2 C1 115.8(5) . . ? C3 N3 C2 115.5(5) . . ? P5 O1 CuA 161.0(3) . . ? C7A O1A CuA 125.9(5) . . ? C4B O1B CuB 124.8(5) . . ? C2C O1C CuC 125.5(4) . . ? C6 O2 P5 123.9(6) . . ? C9A O2A CuA 124.5(5) . . ? C2B O2B CuB 124.0(5) . . ? C4C O2C CuC 124.9(4) . . ? P6 O3 CuB 148.7(3) . . ? C1A O3A CuA 125.5(5) . . ? C9B O3B CuB 124.7(5) . . ? C9C O3C CuC 125.1(5) . . ? C4 O4 P6 127.0(6) . . ? C4A O4A CuA 124.5(5) . . ? C7B O4B CuB 124.0(5) . . ? C7C O4C CuC 124.6(4) . . ? C5 O5 P6 125.6(6) . . ? P4 O6 CuC 163.5(3) . . ? C7 O7 P4 124.3(7) . . ? C8 O8 P4 122.6(5) . . ? C10 O9 P5 125.4(8) . . ? O6 P4 O7 117.5(3) . . ? O6 P4 O8 117.8(3) . . ? O7 P4 O8 98.7(3) . . ? O6 P4 C3 111.1(3) . . ? O7 P4 C3 104.8(3) . . ? O8 P4 C3 105.5(3) . . ? O1 P5 O2 118.2(3) . . ? O1 P5 O9 115.8(3) . . ? O2 P5 O9 100.7(4) . . ? O1 P5 C2 110.2(3) . . ? O2 P5 C2 106.1(3) . . ? O9 P5 C2 104.4(3) . . ? O3 P6 O5 117.1(3) . . ? O3 P6 O4 110.7(3) . . ? O5 P6 O4 108.5(4) . . ? O3 P6 C1 113.0(3) . . ? O5 P6 C1 102.8(3) . . ? O4 P6 C1 103.8(3) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.400 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.056 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 765557' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 Co3 F36 N6 O30 P6' _chemical_formula_weight 2229.49 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' Co Co 0.3494 0.9721 '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' 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' P P 0.1023 0.0942 '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 10.7033(11) _cell_length_b 14.7008(17) _cell_length_c 15.6481(17) _cell_angle_alpha 112.260(13) _cell_angle_beta 98.811(13) _cell_angle_gamma 106.294(13) _cell_volume 2091.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour red-pink _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1107 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6744 _exptl_absorpt_correction_T_max 0.7582 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Rotation, Phi. incr. = 1.5' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20330 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.98 _reflns_number_total 7550 _reflns_number_gt 4532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7550 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7340(4) 0.9948(3) 0.6613(2) 0.0448(8) Uani 1 1 d . . . C1A C 0.6884(5) 0.5905(3) 0.2724(3) 0.0601(10) Uani 1 1 d . . . C1B C 0.8857(4) 1.1592(3) 1.0992(3) 0.0543(9) Uani 1 1 d . . . C2 C 0.6693(4) 0.9643(3) 0.7816(2) 0.0454(8) Uani 1 1 d . . . C2A C 0.7115(5) 0.5462(3) 0.3335(3) 0.0733(13) Uani 1 1 d . . . H2A H 0.7354 0.4870 0.3110 0.088 Uiso 1 1 calc R . . C2B C 0.8200(5) 1.2013(4) 1.1772(3) 0.0698(11) Uani 1 1 d . . . C3 C 0.9707(5) 1.1670(3) 0.6184(3) 0.0798(13) Uani 1 1 d . . . H3A H 0.9782 1.2141 0.5890 0.120 Uiso 1 1 calc R . . H3B H 1.0574 1.1615 0.6357 0.120 Uiso 1 1 calc R . . H3C H 0.9426 1.1939 0.6753 0.120 Uiso 1 1 calc R . . C3A C 0.7013(5) 0.5849(3) 0.4267(3) 0.0638(11) Uani 1 1 d . . . C3B C 0.9888(4) 1.1882(3) 0.9789(3) 0.0565(9) Uani 1 1 d . . . C4 C 0.5728(5) 0.8855(4) 0.9914(3) 0.0794(13) Uani 1 1 d . . . H4A H 0.5229 0.9187 1.0306 0.119 Uiso 1 1 calc R . . H4B H 0.6598 0.8994 1.0318 0.119 Uiso 1 1 calc R . . H4C H 0.5228 0.8105 0.9577 0.119 Uiso 1 1 calc R . . C4A C 0.7446(9) 0.5355(6) 0.4900(4) 0.0969(19) Uani 1 1 d . . . C4B C 1.0282(7) 1.2597(4) 0.9302(4) 0.0801(14) Uani 1 1 d . . . C5A C 0.6976(9) 0.5369(5) 0.1709(4) 0.0966(19) Uani 1 1 d . . . C5B C 0.9217(4) 1.2151(3) 1.0474(3) 0.0634(11) Uani 1 1 d . . . H5B H 0.8992 1.2746 1.0595 0.076 Uiso 1 1 calc R . . C6 C 0.3843(4) 0.9172(3) 0.2586(2) 0.0450(8) Uani 1 1 d . . . C6A C 0.2881(5) 0.5987(3) 0.3284(3) 0.0609(11) Uani 1 1 d . . . C7 C 0.3555(8) 0.6288(4) 0.0936(4) 0.131(2) Uani 1 1 d . . . H7B H 0.2667 0.5806 0.0509 0.197 Uiso 1 1 calc R . . H7C H 0.3939 0.5956 0.1270 0.197 Uiso 1 1 calc R . . H7D H 0.4131 0.6479 0.0569 0.197 Uiso 1 1 calc R . . C7A C 0.2561(4) 0.6645(3) 0.4067(3) 0.0612(10) Uani 1 1 d . . . H7A H 0.1653 0.6518 0.4047 0.073 Uiso 1 1 calc R . . C8A C 0.3566(4) 0.7479(3) 0.4868(2) 0.0503(9) Uani 1 1 d . . . C9 C 0.9734(5) 0.8856(4) 0.6519(4) 0.0879(15) Uani 1 1 d . . . H9A H 1.0646 0.9052 0.6897 0.132 Uiso 1 1 calc R . . H9B H 0.9512 0.8233 0.5927 0.132 Uiso 1 1 calc R . . H9C H 0.9111 0.8716 0.6875 0.132 Uiso 1 1 calc R . . C9A C 0.3119(5) 0.8067(4) 0.5720(3) 0.0714(12) Uani 1 1 d . . . C10 C 0.7136(6) 0.8895(5) 0.2358(4) 0.1041(17) Uani 1 1 d . . . H10A H 0.7614 0.9007 0.1913 0.156 Uiso 1 1 calc R . . H10B H 0.7399 0.8421 0.2564 0.156 Uiso 1 1 calc R . . H10C H 0.7357 0.9559 0.2908 0.156 Uiso 1 1 calc R . . C10A C 0.1665(7) 0.5073(4) 0.2472(4) 0.0888(16) Uani 1 1 d . . . C11 C 0.6313(7) 0.7015(4) 0.7146(4) 0.117(2) Uani 1 1 d . . . H11A H 0.5580 0.6348 0.6746 0.175 Uiso 1 1 calc R . . H11B H 0.7019 0.6909 0.7511 0.175 Uiso 1 1 calc R . . H11C H 0.6671 0.7317 0.6746 0.175 Uiso 1 1 calc R . . Co1 Co 1.0000 1.0000 1.0000 0.0523(2) Uani 1 2 d S . . Co2 Co 0.57848(5) 0.73457(4) 0.40002(3) 0.04824(15) Uani 1 1 d . . . F1 F 0.1804(3) 0.7726(3) 0.5590(2) 0.1174(11) Uani 1 1 d . . . F1B F 0.7250(4) 1.1251(3) 1.1804(3) 0.1254(13) Uani 1 1 d . . . F2 F 0.3723(3) 0.8059(3) 0.65094(18) 0.1106(11) Uani 1 1 d . . . F2B F 0.7686(4) 1.2693(3) 1.1694(3) 0.1321(14) Uani 1 1 d . . . F3 F 0.3485(4) 0.9088(3) 0.5918(2) 0.1165(11) Uani 1 1 d . . . F3B F 0.9093(4) 1.2507(3) 1.26286(19) 0.1070(10) Uani 1 1 d . . . F4A F 0.2088(14) 0.4432(12) 0.1799(11) 0.130(4) Uani 0.50 1 d P . . F4B F 0.9856(18) 1.2090(10) 0.8396(6) 0.148(7) Uani 0.70 1 d P . . F4C F 0.926(3) 1.225(3) 0.849(2) 0.145(16) Uani 0.30 1 d P . . F4D F 0.1802(17) 0.4178(8) 0.2276(17) 0.142(5) Uani 0.50 1 d P . . F5A F 0.0751(19) 0.4599(13) 0.2735(7) 0.195(9) Uani 0.70 1 d P . . F5B F 0.9839(15) 1.3395(9) 0.9583(8) 0.132(5) Uani 0.70 1 d P . . F5C F 1.048(4) 1.3541(16) 0.9759(14) 0.115(11) Uani 0.30 1 d P . . F5D F 0.048(2) 0.497(2) 0.269(3) 0.166(18) Uani 0.30 1 d P . . F6A F 0.1065(15) 0.5352(13) 0.1921(10) 0.137(6) Uani 0.70 1 d P . . F6B F 1.1594(13) 1.3044(10) 0.9574(8) 0.147(5) Uani 0.70 1 d P . . F6C F 1.130(3) 1.257(3) 0.897(3) 0.139(11) Uani 0.30 1 d P . . F6D F 0.155(5) 0.516(4) 0.170(2) 0.21(2) Uani 0.30 1 d P . . F7A F 0.6673(14) 0.5709(8) 0.1145(7) 0.096(4) Uani 0.50 1 d P . . F7B F 0.609(2) 0.5341(18) 0.1063(9) 0.230(12) Uani 0.50 1 d P . . F8 F 0.8308(8) 0.5807(7) 0.1753(4) 0.230(3) Uani 1 1 d . . . F9A F 0.623(2) 0.4326(8) 0.1290(7) 0.202(8) Uani 0.50 1 d P . . F9B F 0.7342(11) 0.4590(7) 0.1539(6) 0.103(3) Uani 0.50 1 d P . . F10A F 0.753(3) 0.4444(13) 0.4426(12) 0.134(8) Uani 0.50 1 d P . . F10B F 0.825(3) 0.489(3) 0.464(2) 0.198(13) Uani 0.50 1 d P . . F11A F 0.867(2) 0.5977(16) 0.5502(18) 0.180(8) Uani 0.50 1 d P . . F11B F 0.801(3) 0.6022(18) 0.5768(10) 0.153(10) Uani 0.50 1 d P . . F12A F 0.6520(17) 0.5101(12) 0.5327(10) 0.139(5) Uani 0.70 1 d P . . F12B F 0.636(4) 0.453(4) 0.471(4) 0.22(2) Uani 0.30 1 d P . . N1 N 0.7303(3) 0.9397(2) 0.71273(19) 0.0494(7) Uani 1 1 d . . . N2 N 0.6772(3) 1.0666(2) 0.67179(18) 0.0472(7) Uani 1 1 d . . . N3 N 0.3893(3) 0.9638(2) 0.19994(19) 0.0472(7) Uani 1 1 d . . . O1 O 0.5723(3) 0.8451(3) 0.1900(2) 0.0747(8) Uani 1 1 d . . . O1A O 0.4004(3) 0.6040(2) 0.31659(18) 0.0642(7) Uani 1 1 d . . . O1B O 0.9049(3) 1.0769(2) 1.09222(18) 0.0602(7) Uani 1 1 d . . . O2 O 0.8717(3) 1.0642(2) 0.55143(18) 0.0626(7) Uani 1 1 d . . . O2A O 0.4821(3) 0.78212(19) 0.50160(16) 0.0536(6) Uani 1 1 d . . . O2B O 1.0247(3) 1.1105(2) 0.94884(19) 0.0663(7) Uani 1 1 d . . . O3 O 0.5925(3) 0.9275(2) 0.92196(18) 0.0638(7) Uani 1 1 d . . . O3A O 0.6604(3) 0.6570(2) 0.46656(18) 0.0700(8) Uani 1 1 d . . . O4 O 0.7523(3) 0.8711(2) 0.48517(17) 0.0624(7) Uani 1 1 d . . . O4A O 0.6560(3) 0.6696(2) 0.28867(17) 0.0605(7) Uani 1 1 d . . . O5 O 0.9634(3) 0.9719(2) 0.63041(19) 0.0633(7) Uani 1 1 d . . . O6 O 0.8122(3) 0.9028(2) 0.89219(18) 0.0670(7) Uani 1 1 d . . . O7 O 0.5811(3) 0.7732(2) 0.78061(19) 0.0675(7) Uani 1 1 d . . . O8 O 0.5112(3) 0.81491(19) 0.32969(17) 0.0604(7) Uani 1 1 d . . . O9 O 0.3451(3) 0.7200(2) 0.1608(2) 0.0861(10) Uani 1 1 d . . . P1 P 0.82937(10) 0.96764(8) 0.57329(6) 0.0494(2) Uani 1 1 d . . . P2 P 0.67309(10) 0.88937(8) 0.85108(6) 0.0499(2) Uani 1 1 d . . . P3 P 0.46327(11) 0.81909(7) 0.24007(6) 0.0515(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 C1 0.043(2) 0.054(2) 0.0327(16) 0.0147(15) 0.0102(14) 0.0189(17) C1A 0.083(3) 0.052(2) 0.051(2) 0.0193(18) 0.033(2) 0.031(2) C1B 0.044(2) 0.066(2) 0.049(2) 0.0222(19) 0.0092(17) 0.0219(19) C2 0.045(2) 0.054(2) 0.0339(17) 0.0154(15) 0.0104(15) 0.0209(17) C2A 0.118(4) 0.064(3) 0.061(2) 0.028(2) 0.040(3) 0.059(3) C2B 0.067(3) 0.073(3) 0.066(3) 0.024(2) 0.024(2) 0.028(2) C3 0.092(4) 0.068(3) 0.073(3) 0.031(2) 0.023(3) 0.020(3) C3A 0.085(3) 0.063(2) 0.057(2) 0.031(2) 0.025(2) 0.039(2) C3B 0.055(3) 0.064(2) 0.043(2) 0.0253(19) 0.0049(17) 0.015(2) C4 0.098(4) 0.096(3) 0.067(3) 0.053(3) 0.042(3) 0.037(3) C4A 0.155(7) 0.100(5) 0.072(4) 0.048(3) 0.041(4) 0.080(5) C4B 0.102(5) 0.074(3) 0.070(3) 0.040(3) 0.029(3) 0.027(3) C5A 0.162(7) 0.093(4) 0.083(4) 0.047(3) 0.084(4) 0.077(4) C5B 0.073(3) 0.060(2) 0.057(2) 0.025(2) 0.015(2) 0.028(2) C6 0.054(2) 0.0478(19) 0.0300(16) 0.0142(14) 0.0111(15) 0.0201(17) C6A 0.076(3) 0.050(2) 0.044(2) 0.0187(18) 0.005(2) 0.016(2) C7 0.180(7) 0.082(4) 0.080(4) -0.012(3) 0.047(4) 0.038(4) C7A 0.051(3) 0.064(2) 0.058(2) 0.024(2) 0.0076(19) 0.017(2) C8A 0.058(3) 0.055(2) 0.0413(19) 0.0214(17) 0.0127(18) 0.027(2) C9 0.085(4) 0.096(3) 0.117(4) 0.061(3) 0.038(3) 0.058(3) C9A 0.057(3) 0.092(3) 0.060(3) 0.021(2) 0.022(2) 0.037(3) C10 0.073(4) 0.122(5) 0.118(5) 0.063(4) 0.030(3) 0.022(3) C10A 0.093(5) 0.069(3) 0.068(3) 0.017(3) -0.003(3) 0.011(3) C11 0.157(6) 0.069(3) 0.110(4) 0.018(3) 0.049(4) 0.046(4) Co1 0.0543(5) 0.0766(5) 0.0480(4) 0.0380(4) 0.0215(3) 0.0370(4) Co2 0.0650(4) 0.0507(3) 0.0349(2) 0.0177(2) 0.0203(2) 0.0286(2) F1 0.064(2) 0.163(3) 0.088(2) 0.014(2) 0.0342(16) 0.043(2) F1B 0.118(3) 0.094(2) 0.140(3) 0.019(2) 0.090(2) 0.024(2) F2 0.110(3) 0.190(3) 0.0520(15) 0.0486(18) 0.0412(15) 0.083(2) F2B 0.177(4) 0.166(3) 0.139(3) 0.085(3) 0.092(3) 0.136(3) F3 0.133(3) 0.089(2) 0.112(2) 0.0108(18) 0.047(2) 0.062(2) F3B 0.127(3) 0.120(2) 0.0577(16) 0.0204(16) 0.0317(17) 0.047(2) F4A 0.149(8) 0.081(8) 0.076(7) -0.022(5) 0.002(6) 0.022(7) F4B 0.28(2) 0.087(4) 0.046(4) 0.039(4) 0.026(8) 0.029(11) F4C 0.120(14) 0.15(3) 0.12(2) 0.10(2) -0.050(13) -0.024(12) F4D 0.134(11) 0.050(4) 0.159(13) -0.002(6) -0.031(9) 0.022(5) F5A 0.209(17) 0.132(10) 0.101(6) 0.031(6) 0.008(7) -0.091(9) F5B 0.185(12) 0.113(8) 0.154(9) 0.098(8) 0.065(8) 0.072(8) F5C 0.20(3) 0.046(7) 0.061(7) 0.005(6) 0.055(12) 0.017(11) F5D 0.041(9) 0.116(17) 0.20(3) -0.042(16) 0.025(11) -0.001(10) F6A 0.105(8) 0.137(6) 0.112(9) 0.039(6) -0.036(6) 0.023(6) F6B 0.124(7) 0.155(9) 0.152(8) 0.100(7) 0.043(7) -0.008(6) F6C 0.15(2) 0.18(3) 0.22(3) 0.16(3) 0.14(2) 0.09(2) F6D 0.22(4) 0.21(4) 0.068(13) 0.09(2) -0.058(17) -0.10(3) F7A 0.183(11) 0.098(4) 0.056(5) 0.049(4) 0.073(7) 0.080(5) F7B 0.28(2) 0.36(3) 0.035(5) 0.002(9) 0.014(8) 0.25(2) F8 0.261(8) 0.367(10) 0.183(5) 0.155(6) 0.170(5) 0.186(7) F9A 0.39(2) 0.065(5) 0.070(6) -0.002(4) 0.092(11) 0.006(10) F9B 0.201(9) 0.082(6) 0.071(5) 0.028(4) 0.074(6) 0.103(7) F10A 0.28(3) 0.103(7) 0.116(7) 0.081(6) 0.110(12) 0.136(12) F10B 0.28(3) 0.29(3) 0.22(2) 0.19(2) 0.139(19) 0.24(3) F11A 0.172(15) 0.153(15) 0.173(17) 0.064(15) -0.062(12) 0.070(10) F11B 0.25(3) 0.184(16) 0.080(6) 0.066(8) 0.025(10) 0.16(2) F12A 0.208(13) 0.193(11) 0.134(7) 0.135(8) 0.097(9) 0.126(11) F12B 0.22(3) 0.21(3) 0.21(3) 0.18(3) -0.03(3) -0.02(2) N1 0.054(2) 0.0595(18) 0.0412(15) 0.0229(14) 0.0174(14) 0.0284(15) N2 0.057(2) 0.0509(16) 0.0358(14) 0.0182(13) 0.0153(13) 0.0234(15) N3 0.0509(19) 0.0558(17) 0.0359(14) 0.0180(13) 0.0151(13) 0.0232(14) O1 0.084(2) 0.112(2) 0.0658(17) 0.0513(17) 0.0428(16) 0.063(2) O1A 0.078(2) 0.0517(15) 0.0500(15) 0.0116(12) 0.0191(14) 0.0208(15) O1B 0.0622(18) 0.0824(19) 0.0576(15) 0.0389(14) 0.0292(13) 0.0400(15) O2 0.0689(19) 0.0732(18) 0.0533(15) 0.0352(14) 0.0233(13) 0.0244(15) O2A 0.0531(18) 0.0622(15) 0.0392(13) 0.0149(12) 0.0157(12) 0.0219(13) O2B 0.077(2) 0.087(2) 0.0620(16) 0.0482(16) 0.0304(15) 0.0409(17) O3 0.075(2) 0.0883(19) 0.0583(15) 0.0467(15) 0.0373(14) 0.0432(16) O3A 0.109(2) 0.0723(18) 0.0468(15) 0.0281(14) 0.0296(15) 0.0527(18) O4 0.0603(18) 0.0715(17) 0.0426(14) 0.0135(13) 0.0210(12) 0.0200(14) O4A 0.092(2) 0.0598(15) 0.0489(14) 0.0272(12) 0.0362(14) 0.0428(15) O5 0.0576(18) 0.0776(18) 0.0598(16) 0.0316(14) 0.0184(13) 0.0303(14) O6 0.0633(19) 0.093(2) 0.0544(15) 0.0389(15) 0.0128(13) 0.0365(16) O7 0.074(2) 0.0607(16) 0.0627(17) 0.0262(14) 0.0155(15) 0.0212(15) O8 0.086(2) 0.0617(15) 0.0506(14) 0.0288(13) 0.0253(14) 0.0435(15) O9 0.094(3) 0.0598(17) 0.0677(19) -0.0040(15) 0.0101(17) 0.0298(17) P1 0.0511(6) 0.0614(6) 0.0395(5) 0.0213(4) 0.0187(4) 0.0246(5) P2 0.0539(6) 0.0625(6) 0.0419(5) 0.0277(4) 0.0155(4) 0.0268(5) P3 0.0680(7) 0.0522(5) 0.0380(5) 0.0163(4) 0.0188(4) 0.0312(5) _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 C1 N2 1.330(4) . ? C1 N1 1.338(4) . ? C1 P1 1.828(3) . ? C1A O4A 1.251(4) . ? C1A C2A 1.374(5) . ? C1A C5A 1.516(6) . ? C1B O1B 1.251(4) . ? C1B C5B 1.379(5) . ? C1B C2B 1.517(6) . ? C2 N1 1.332(4) . ? C2 N3 1.338(4) 2_676 ? C2 P2 1.821(3) . ? C2A C3A 1.385(5) . ? C2A H2A 0.9300 . ? C2B F2B 1.303(5) . ? C2B F1B 1.307(5) . ? C2B F3B 1.311(5) . ? C3 O2 1.438(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3A O3A 1.244(4) . ? C3A C4A 1.522(6) . ? C3B O2B 1.251(5) . ? C3B C5B 1.377(6) . ? C3B C4B 1.523(6) . ? C4 O3 1.453(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4A F11B 1.256(19) . ? C4A F10B 1.26(2) . ? C4A F10A 1.297(14) . ? C4A F11A 1.32(2) . ? C4A F12B 1.32(3) . ? C4A F12A 1.323(13) . ? C4B F5C 1.23(2) . ? C4B F4B 1.259(10) . ? C4B F6C 1.28(2) . ? C4B F6B 1.294(13) . ? C4B F5B 1.334(13) . ? C4B F4C 1.36(2) . ? C5A F7A 1.212(11) . ? C5A F7B 1.256(16) . ? C5A F9B 1.261(8) . ? C5A F9A 1.345(11) . ? C5A F8 1.369(9) . ? C5B H5B 0.9300 . ? C6 N2 1.337(4) 2_676 ? C6 N3 1.338(4) . ? C6 P3 1.822(3) . ? C6A O1A 1.229(5) . ? C6A C7A 1.404(6) . ? C6A C10A 1.528(6) . ? C7 O9 1.402(6) . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7D 0.9600 . ? C7A C8A 1.383(5) . ? C7A H7A 0.9300 . ? C8A O2A 1.245(4) . ? C8A C9A 1.518(5) . ? C9 O5 1.456(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C9A F1 1.308(5) . ? C9A F2 1.309(5) . ? C9A F3 1.335(5) . ? C10 O1 1.409(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10A F6D 1.25(2) . ? C10A F5A 1.253(13) . ? C10A F6A 1.253(11) . ? C10A F4D 1.290(11) . ? C10A F5D 1.35(2) . ? C10A F4A 1.355(13) . ? C11 O7 1.460(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? Co1 O2B 2.040(2) 2_777 ? Co1 O2B 2.040(2) . ? Co1 O1B 2.063(2) . ? Co1 O1B 2.063(3) 2_777 ? Co1 O6 2.109(3) . ? Co1 O6 2.109(3) 2_777 ? Co2 O2A 2.036(2) . ? Co2 O4A 2.065(2) . ? Co2 O1A 2.076(3) . ? Co2 O3A 2.081(2) . ? Co2 O8 2.084(2) . ? Co2 O4 2.094(3) . ? F4A F4D 1.003(15) . ? F4A F6D 1.39(5) . ? F4B F4C 0.75(4) . ? F4B F6C 1.48(3) . ? F4C F5B 1.75(3) . ? F4D F5A 1.570(18) . ? F5A F5D 0.71(3) . ? F5B F5C 0.64(4) . ? F5C F6B 1.57(3) . ? F5D F6A 1.65(4) . ? F6A F6D 0.73(7) . ? F6B F6C 0.87(3) . ? F7A F7B 0.66(3) . ? F7B F9A 1.70(2) . ? F8 F9B 1.669(12) . ? F9A F9B 1.098(17) . ? F10A F10B 0.79(4) . ? F10A F12B 1.41(5) . ? F10B F11A 1.53(3) . ? F11A F11B 0.88(3) . ? F11B F12A 1.61(3) . ? F12A F12B 0.97(5) . ? N2 C6 1.337(4) 2_676 ? N3 C2 1.338(4) 2_676 ? O1 P3 1.542(3) . ? O2 P1 1.546(3) . ? O3 P2 1.543(3) . ? O4 P1 1.452(3) . ? O5 P1 1.541(3) . ? O6 P2 1.455(3) . ? O7 P2 1.549(3) . ? O8 P3 1.448(2) . ? O9 P3 1.542(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 N2 C1 N1 125.0(3) . . ? N2 C1 P1 120.0(2) . . ? N1 C1 P1 114.9(2) . . ? O4A C1A C2A 128.1(3) . . ? O4A C1A C5A 114.1(3) . . ? C2A C1A C5A 117.7(4) . . ? O1B C1B C5B 127.4(4) . . ? O1B C1B C2B 113.8(3) . . ? C5B C1B C2B 118.7(4) . . ? N1 C2 N3 125.0(3) . 2_676 ? N1 C2 P2 112.9(2) . . ? N3 C2 P2 122.1(3) 2_676 . ? C1A C2A C3A 123.5(3) . . ? C1A C2A H2A 118.2 . . ? C3A C2A H2A 118.2 . . ? F2B C2B F1B 108.5(4) . . ? F2B C2B F3B 105.8(4) . . ? F1B C2B F3B 105.4(4) . . ? F2B C2B C1B 114.0(4) . . ? F1B C2B C1B 111.9(4) . . ? F3B C2B C1B 110.8(4) . . ? O2 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3A C3A C2A 127.6(3) . . ? O3A C3A C4A 114.5(4) . . ? C2A C3A C4A 117.9(4) . . ? O2B C3B C5B 129.0(4) . . ? O2B C3B C4B 112.3(4) . . ? C5B C3B C4B 118.6(4) . . ? O3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? F11B C4A F10B 107.2(16) . . ? F11B C4A F10A 130.2(11) . . ? F10B C4A F10A 35.7(17) . . ? F11B C4A F11A 39.9(12) . . ? F10B C4A F11A 72.9(15) . . ? F10A C4A F11A 106.0(14) . . ? F11B C4A F12B 118(2) . . ? F10B C4A F12B 100(2) . . ? F10A C4A F12B 65(3) . . ? F11A C4A F12B 144.1(13) . . ? F11B C4A F12A 77.2(11) . . ? F10B C4A F12A 127.4(13) . . ? F10A C4A F12A 101.1(11) . . ? F11A C4A F12A 114.0(12) . . ? F12B C4A F12A 43(2) . . ? F11B C4A C3A 112.3(9) . . ? F10B C4A C3A 114.0(10) . . ? F10A C4A C3A 114.1(8) . . ? F11A C4A C3A 109.7(10) . . ? F12B C4A C3A 105.5(12) . . ? F12A C4A C3A 111.7(7) . . ? F5C C4B F4B 124.6(13) . . ? F5C C4B F6C 105.8(19) . . ? F4B C4B F6C 71.3(16) . . ? F5C C4B F6B 77.0(17) . . ? F4B C4B F6B 109.6(10) . . ? F6C C4B F6B 39.4(16) . . ? F5C C4B F5B 28.5(19) . . ? F4B C4B F5B 109.1(9) . . ? F6C C4B F5B 126.9(13) . . ? F6B C4B F5B 105.0(9) . . ? F5C C4B F4C 105(2) . . ? F4B C4B F4C 33.2(17) . . ? F6C C4B F4C 102(2) . . ? F6B C4B F4C 135.9(16) . . ? F5B C4B F4C 80.9(16) . . ? F5C C4B C3B 117.7(11) . . ? F4B C4B C3B 111.9(7) . . ? F6C C4B C3B 115.9(10) . . ? F6B C4B C3B 108.4(6) . . ? F5B C4B C3B 112.6(7) . . ? F4C C4B C3B 109.1(16) . . ? F7A C5A F7B 30.8(13) . . ? F7A C5A F9B 126.8(7) . . ? F7B C5A F9B 119.4(10) . . ? F7A C5A F9A 107.2(10) . . ? F7B C5A F9A 81.5(13) . . ? F9B C5A F9A 49.7(8) . . ? F7A C5A F8 88.1(7) . . ? F7B C5A F8 117.1(12) . . ? F9B C5A F8 78.6(7) . . ? F9A C5A F8 125.2(10) . . ? F7A C5A C1A 118.0(6) . . ? F7B C5A C1A 114.7(9) . . ? F9B C5A C1A 115.1(6) . . ? F9A C5A C1A 111.1(6) . . ? F8 C5A C1A 106.1(6) . . ? C3B C5B C1B 124.0(4) . . ? C3B C5B H5B 118.0 . . ? C1B C5B H5B 118.0 . . ? N2 C6 N3 126.0(3) 2_676 . ? N2 C6 P3 116.6(2) 2_676 . ? N3 C6 P3 117.4(2) . . ? O1A C6A C7A 129.0(4) . . ? O1A C6A C10A 115.6(4) . . ? C7A C6A C10A 115.4(5) . . ? O9 C7 H7B 109.5 . . ? O9 C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O9 C7 H7D 109.5 . . ? H7B C7 H7D 109.5 . . ? H7C C7 H7D 109.5 . . ? C8A C7A C6A 121.5(4) . . ? C8A C7A H7A 119.3 . . ? C6A C7A H7A 119.3 . . ? O2A C8A C7A 129.5(4) . . ? O2A C8A C9A 113.2(3) . . ? C7A C8A C9A 117.3(4) . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F1 C9A F2 108.7(4) . . ? F1 C9A F3 105.5(4) . . ? F2 C9A F3 105.2(4) . . ? F1 C9A C8A 114.8(4) . . ? F2 C9A C8A 111.5(3) . . ? F3 C9A C8A 110.5(4) . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F6D C10A F5A 128(2) . . ? F6D C10A F6A 34(3) . . ? F5A C10A F6A 105.0(11) . . ? F6D C10A F4D 105(3) . . ? F5A C10A F4D 76.3(10) . . ? F6A C10A F4D 128.9(11) . . ? F6D C10A F5D 109(2) . . ? F5A C10A F5D 31.2(16) . . ? F6A C10A F5D 78(2) . . ? F4D C10A F5D 105.7(14) . . ? F6D C10A F4A 64(3) . . ? F5A C10A F4A 114.6(10) . . ? F6A C10A F4A 96.0(10) . . ? F4D C10A F4A 44.5(8) . . ? F5D C10A F4A 134.4(11) . . ? F6D C10A C6A 111.8(16) . . ? F5A C10A C6A 115.7(6) . . ? F6A C10A C6A 113.0(8) . . ? F4D C10A C6A 111.5(7) . . ? F5D C10A C6A 113.1(12) . . ? F4A C10A C6A 110.7(7) . . ? O7 C11 H11A 109.5 . . ? O7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2B Co1 O2B 180.00 2_777 . ? O2B Co1 O1B 90.86(10) 2_777 . ? O2B Co1 O1B 89.14(10) . . ? O2B Co1 O1B 89.14(10) 2_777 2_777 ? O2B Co1 O1B 90.86(11) . 2_777 ? O1B Co1 O1B 180.00 . 2_777 ? O2B Co1 O6 89.30(11) 2_777 . ? O2B Co1 O6 90.70(11) . . ? O1B Co1 O6 91.18(11) . . ? O1B Co1 O6 88.82(11) 2_777 . ? O2B Co1 O6 90.70(11) 2_777 2_777 ? O2B Co1 O6 89.30(11) . 2_777 ? O1B Co1 O6 88.82(11) . 2_777 ? O1B Co1 O6 91.18(11) 2_777 2_777 ? O6 Co1 O6 180.00 . 2_777 ? O2A Co2 O4A 173.11(11) . . ? O2A Co2 O1A 88.28(11) . . ? O4A Co2 O1A 84.91(12) . . ? O2A Co2 O3A 92.51(10) . . ? O4A Co2 O3A 86.95(10) . . ? O1A Co2 O3A 94.07(12) . . ? O2A Co2 O8 91.58(10) . . ? O4A Co2 O8 89.29(9) . . ? O1A Co2 O8 88.62(11) . . ? O3A Co2 O8 175.17(12) . . ? O2A Co2 O4 89.82(10) . . ? O4A Co2 O4 97.02(11) . . ? O1A Co2 O4 177.14(11) . . ? O3A Co2 O4 88.15(12) . . ? O8 Co2 O4 89.29(11) . . ? F4D F4A C10A 64.3(11) . . ? F4D F4A F6D 114(3) . . ? C10A F4A F6D 54.2(17) . . ? F4C F4B C4B 81(3) . . ? F4C F4B F6C 131(3) . . ? C4B F4B F6C 55.0(10) . . ? F4B F4C C4B 66(2) . . ? F4B F4C F5B 109(3) . . ? C4B F4C F5B 48.9(10) . . ? F4A F4D C10A 71.2(12) . . ? F4A F4D F5A 115.3(16) . . ? C10A F4D F5A 50.8(7) . . ? F5D F5A C10A 82(3) . . ? F5D F5A F4D 131(4) . . ? C10A F5A F4D 52.9(7) . . ? F5C F5B C4B 67(3) . . ? F5C F5B F4C 110(3) . . ? C4B F5B F4C 50.2(10) . . ? F5B F5C C4B 85(3) . . ? F5B F5C F6B 137(3) . . ? C4B F5C F6B 53.3(11) . . ? F5A F5D C10A 67(2) . . ? F5A F5D F6A 109(4) . . ? C10A F5D F6A 48.3(14) . . ? F6D F6A C10A 73(3) . . ? F6D F6A F5D 121(3) . . ? C10A F6A F5D 53.3(10) . . ? F6C F6B C4B 69(2) . . ? F6C F6B F5C 107(2) . . ? C4B F6B F5C 49.7(11) . . ? F6B F6C C4B 71.2(19) . . ? F6B F6C F4B 123(3) . . ? C4B F6C F4B 53.7(11) . . ? F6A F6D C10A 73(3) . . ? F6A F6D F4A 130(4) . . ? C10A F6D F4A 61.5(16) . . ? F7B F7A C5A 78.3(18) . . ? F7A F7B C5A 71(2) . . ? F7A F7B F9A 115(3) . . ? C5A F7B F9A 51.5(9) . . ? C5A F8 F9B 47.8(4) . . ? F9B F9A C5A 61.2(8) . . ? F9B F9A F7B 99.8(12) . . ? C5A F9A F7B 47.0(8) . . ? F9A F9B C5A 69.1(8) . . ? F9A F9B F8 119.7(10) . . ? C5A F9B F8 53.5(5) . . ? F10B F10A C4A 70(2) . . ? F10B F10A F12B 126(3) . . ? C4A F10A F12B 58.3(16) . . ? F10A F10B C4A 74(3) . . ? F10A F10B F11A 125(3) . . ? C4A F10B F11A 55.2(11) . . ? F11B F11A C4A 66(2) . . ? F11B F11A F10B 111(3) . . ? C4A F11A F10B 51.9(12) . . ? F11A F11B C4A 73.8(19) . . ? F11A F11B F12A 123(3) . . ? C4A F11B F12A 53.3(11) . . ? F12B F12A C4A 68(2) . . ? F12B F12A F11B 116(3) . . ? C4A F12A F11B 49.5(7) . . ? F12A F12B C4A 69(2) . . ? F12A F12B F10A 116(3) . . ? C4A F12B F10A 56.7(17) . . ? C2 N1 C1 115.4(3) . . ? C1 N2 C6 114.4(3) . 2_676 ? C6 N3 C2 114.2(3) . 2_676 ? C10 O1 P3 124.2(3) . . ? C6A O1A Co2 123.8(3) . . ? C1B O1B Co1 125.5(2) . . ? C3 O2 P1 124.7(2) . . ? C8A O2A Co2 124.6(2) . . ? C3B O2B Co1 124.8(3) . . ? C4 O3 P2 120.4(3) . . ? C3A O3A Co2 125.6(2) . . ? P1 O4 Co2 152.19(17) . . ? C1A O4A Co2 124.7(2) . . ? C9 O5 P1 122.8(3) . . ? P2 O6 Co1 147.75(18) . . ? C11 O7 P2 122.1(3) . . ? P3 O8 Co2 148.76(16) . . ? C7 O9 P3 126.8(4) . . ? O4 P1 O5 116.22(16) . . ? O4 P1 O2 110.83(15) . . ? O5 P1 O2 104.74(16) . . ? O4 P1 C1 112.85(16) . . ? O5 P1 C1 104.01(15) . . ? O2 P1 C1 107.47(15) . . ? O6 P2 O3 117.43(16) . . ? O6 P2 O7 113.51(17) . . ? O3 P2 O7 104.92(17) . . ? O6 P2 C2 110.67(17) . . ? O3 P2 C2 103.37(14) . . ? O7 P2 C2 105.87(15) . . ? O8 P3 O9 116.54(18) . . ? O8 P3 O1 115.69(17) . . ? O9 P3 O1 105.40(19) . . ? O8 P3 C6 110.82(14) . . ? O9 P3 C6 100.10(17) . . ? O1 P3 C6 106.78(16) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.489 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.066 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 765558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 F36 Mn3 N6 O30 P6' _chemical_formula_weight 2217.52 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' F F 0.0171 0.0103 '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' 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' P P 0.1023 0.0942 '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 10.7403(5) _cell_length_b 14.6581(4) _cell_length_c 15.8125(7) _cell_angle_alpha 112.201(6) _cell_angle_beta 97.921(7) _cell_angle_gamma 107.180(5) _cell_volume 2112.66(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 237 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1101 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27032 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7419 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1257P)^2^+1.1763P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7419 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.2111 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 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 C1 C 0.7369(5) 1.0023(4) 0.6672(4) 0.0397(13) Uani 1 1 d . . . C1A C 0.6848(7) 0.5811(5) 0.2669(5) 0.0561(16) Uani 1 1 d . . . C1B C 0.8828(6) 1.1626(5) 1.1034(5) 0.0535(16) Uani 1 1 d . . . C2 C 0.6680(5) 0.9647(5) 0.7829(4) 0.0438(13) Uani 1 1 d . . . C2A C 0.7133(8) 0.5395(6) 0.3281(5) 0.069(2) Uani 1 1 d . . . H2A H 0.7348 0.4793 0.3060 0.082 Uiso 1 1 calc R . . C2B C 0.8165(8) 1.2014(6) 1.1834(6) 0.0667(19) Uani 1 1 d . . . C3 C 0.9819(8) 1.1837(6) 0.6315(6) 0.086(2) Uani 1 1 d . . . H3A H 0.9920 1.2331 0.6043 0.129 Uiso 1 1 calc R . . H3B H 1.0669 1.1762 0.6466 0.129 Uiso 1 1 calc R . . H3C H 0.9546 1.2097 0.6884 0.129 Uiso 1 1 calc R . . C3A C 0.7110(8) 0.5844(6) 0.4224(5) 0.0649(18) Uani 1 1 d . . . C3B C 0.9824(7) 1.1978(6) 0.9845(5) 0.0578(17) Uani 1 1 d . . . C4 C 0.5634(9) 0.8798(7) 0.9867(6) 0.086(2) Uani 1 1 d . . . H4A H 0.5135 0.9136 1.0252 0.129 Uiso 1 1 calc R . . H4B H 0.6494 0.8940 1.0265 0.129 Uiso 1 1 calc R . . H4C H 0.5126 0.8044 0.9539 0.129 Uiso 1 1 calc R . . C4A C 0.7590(15) 0.5370(10) 0.4859(8) 0.104(3) Uani 1 1 d . . . C4B C 1.0172(10) 1.2724(7) 0.9386(6) 0.081(2) Uani 1 1 d . . . C5A C 0.6785(14) 0.5190(9) 0.1631(7) 0.104(3) Uani 1 1 d . . . C5B C 0.9141(7) 1.2221(5) 1.0537(5) 0.0607(17) Uani 1 1 d . . . H5B H 0.8888 1.2803 1.0668 0.073 Uiso 1 1 calc R . . C6 C 0.3860(6) 0.9155(4) 0.2531(4) 0.0440(14) Uani 1 1 d . . . C6A C 0.2824(7) 0.5991(5) 0.3343(4) 0.0560(17) Uani 1 1 d . . . C7 C 0.3562(11) 0.6244(7) 0.0996(7) 0.114(3) Uani 1 1 d . . . H7B H 0.2677 0.5764 0.0571 0.171 Uiso 1 1 calc R . . H7C H 0.3876 0.5934 0.1375 0.171 Uiso 1 1 calc R . . H7D H 0.4182 0.6375 0.0633 0.171 Uiso 1 1 calc R . . C7A C 0.2527(7) 0.6655(5) 0.4109(5) 0.0588(17) Uani 1 1 d . . . H7A H 0.1622 0.6530 0.4097 0.071 Uiso 1 1 calc R . . C8A C 0.3523(6) 0.7492(5) 0.4888(4) 0.0491(15) Uani 1 1 d . . . C9 C 0.9730(8) 0.8910(7) 0.6475(7) 0.089(3) Uani 1 1 d . . . H9A H 1.0626 0.9086 0.6848 0.133 Uiso 1 1 calc R . . H9B H 0.9530 0.8326 0.5864 0.133 Uiso 1 1 calc R . . H9C H 0.9080 0.8711 0.6797 0.133 Uiso 1 1 calc R . . C9A C 0.3101(8) 0.8113(7) 0.5731(5) 0.072(2) Uani 1 1 d . . . C10 C 0.7125(9) 0.8859(10) 0.2215(8) 0.125(4) Uani 1 1 d . . . H10A H 0.7572 0.8963 0.1755 0.187 Uiso 1 1 calc R . . H10B H 0.7354 0.8352 0.2383 0.187 Uiso 1 1 calc R . . H10C H 0.7416 0.9524 0.2774 0.187 Uiso 1 1 calc R . . C10A C 0.1592(11) 0.5067(7) 0.2547(6) 0.090(3) Uani 1 1 d . . . C11 C 0.6290(11) 0.6986(7) 0.7107(8) 0.118(4) Uani 1 1 d . . . H11A H 0.5551 0.6318 0.6708 0.178 Uiso 1 1 calc R . . H11B H 0.6983 0.6870 0.7456 0.178 Uiso 1 1 calc R . . H11C H 0.6659 0.7302 0.6719 0.178 Uiso 1 1 calc R . . F1 F 0.1778(4) 0.7758(5) 0.5605(3) 0.117(2) Uani 1 1 d . . . F1B F 0.7178(5) 1.1234(4) 1.1808(4) 0.126(2) Uani 1 1 d . . . F2 F 0.3683(5) 0.8095(5) 0.6510(3) 0.1135(19) Uani 1 1 d . . . F2B F 0.7694(7) 1.2731(5) 1.1810(4) 0.129(2) Uani 1 1 d . . . F3 F 0.3500(6) 0.9133(4) 0.5919(4) 0.118(2) Uani 1 1 d . . . F3B F 0.9062(5) 1.2464(4) 1.2665(3) 0.1042(16) Uani 1 1 d . . . F4A F 0.2066(18) 0.4512(16) 0.1813(11) 0.147(9) Uani 0.50 1 d P . . F4C F 0.9565(10) 1.2245(5) 0.8497(4) 0.184(4) Uani 1 1 d . . . F4D F 0.1734(17) 0.4182(11) 0.2273(19) 0.137(8) Uani 0.50 1 d P . . F5A F 0.074(2) 0.4591(19) 0.2827(13) 0.239(15) Uani 0.70 1 d P . . F5B F 0.9902(9) 1.3573(5) 0.9724(5) 0.152(3) Uani 1 1 d . . . F5D F 0.040(2) 0.493(3) 0.270(3) 0.130(17) Uani 0.30 1 d P . . F6A F 0.1112(9) 0.5358(7) 0.1967(6) 0.174(3) Uani 1 1 d . . . F6C F 1.1439(8) 1.3105(7) 0.9503(7) 0.196(4) Uani 1 1 d . . . F7A F 0.6457(9) 0.5543(6) 0.1066(4) 0.152(3) Uani 1 1 d . . . F8 F 0.8062(13) 0.5407(15) 0.1569(7) 0.280(8) Uani 1 1 d . . . F9A F 0.558(2) 0.4377(14) 0.1184(9) 0.204(11) Uani 0.50 1 d P . . F9B F 0.690(2) 0.4315(10) 0.1407(8) 0.114(5) Uani 0.50 1 d P . . F10A F 0.7834(13) 0.4551(8) 0.4442(6) 0.214(5) Uani 1 1 d . . . F11A F 0.886(2) 0.596(2) 0.536(2) 0.195(12) Uani 0.50 1 d P . . F11B F 0.812(3) 0.6007(19) 0.5700(11) 0.142(10) Uani 0.50 1 d P . . F12A F 0.6555(13) 0.5017(10) 0.5190(9) 0.205(4) Uani 1 1 d . . . Mn1 Mn 1.0000 1.0000 1.0000 0.0546(4) Uani 1 2 d S . . Mn2 Mn 0.58639(9) 0.74116(7) 0.40088(6) 0.0434(3) Uani 1 1 d . . . N1 N 0.7335(5) 0.9448(4) 0.7156(3) 0.0424(11) Uani 1 1 d . . . N2 N 0.6779(5) 1.0723(4) 0.6781(3) 0.0444(11) Uani 1 1 d . . . N3 N 0.3927(5) 0.9655(4) 0.1981(3) 0.0441(11) Uani 1 1 d . . . O1 O 0.5739(5) 0.8483(5) 0.1835(4) 0.0781(15) Uani 1 1 d . . . O1A O 0.3949(5) 0.6037(3) 0.3219(3) 0.0641(12) Uani 1 1 d . . . O1B O 0.9020(5) 1.0812(4) 1.0952(3) 0.0642(12) Uani 1 1 d . . . O2 O 0.8804(4) 1.0822(4) 0.5643(3) 0.0613(12) Uani 1 1 d . . . O2A O 0.4788(4) 0.7826(3) 0.5035(3) 0.0533(11) Uani 1 1 d . . . O2B O 1.0205(5) 1.1220(4) 0.9541(3) 0.0705(13) Uani 1 1 d . . . O3 O 0.5855(5) 0.9215(4) 0.9177(3) 0.0655(12) Uani 1 1 d . . . O3A O 0.6814(5) 0.6611(4) 0.4635(3) 0.0684(13) Uani 1 1 d . . . O4 O 0.7564(4) 0.8867(3) 0.4920(3) 0.0568(11) Uani 1 1 d . . . O4A O 0.6591(5) 0.6631(3) 0.2832(3) 0.0574(11) Uani 1 1 d . . . O5 O 0.9661(4) 0.9815(4) 0.6351(3) 0.0618(12) Uani 1 1 d . . . O6 O 0.8072(4) 0.9024(4) 0.8914(3) 0.0669(13) Uani 1 1 d . . . O7 O 0.5799(5) 0.7694(4) 0.7768(3) 0.0693(13) Uani 1 1 d . . . O8 O 0.5200(5) 0.8162(3) 0.3219(3) 0.0592(11) Uani 1 1 d . . . O9 O 0.3492(5) 0.7191(4) 0.1582(4) 0.0889(17) Uani 1 1 d . . . P1 P 0.83411(15) 0.98081(13) 0.58049(11) 0.0465(4) Uani 1 1 d . . . P2 P 0.66910(16) 0.88666(14) 0.84864(11) 0.0486(4) Uani 1 1 d . . . P3 P 0.46819(18) 0.82013(13) 0.23442(11) 0.0509(4) 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 C1 0.040(3) 0.046(3) 0.029(3) 0.015(3) 0.006(2) 0.014(3) C1A 0.080(5) 0.047(4) 0.048(4) 0.021(3) 0.031(3) 0.029(3) C1B 0.041(3) 0.064(4) 0.052(4) 0.024(3) 0.008(3) 0.020(3) C2 0.040(3) 0.056(4) 0.041(3) 0.024(3) 0.009(3) 0.021(3) C2A 0.109(6) 0.059(4) 0.063(5) 0.031(4) 0.036(4) 0.055(4) C2B 0.060(4) 0.066(5) 0.071(5) 0.024(4) 0.025(4) 0.027(4) C3 0.092(6) 0.068(5) 0.083(6) 0.038(5) 0.014(5) 0.009(4) C3A 0.089(5) 0.067(5) 0.059(4) 0.036(4) 0.021(4) 0.046(4) C3B 0.057(4) 0.062(4) 0.048(4) 0.030(3) -0.001(3) 0.012(3) C4 0.103(6) 0.107(6) 0.080(5) 0.066(5) 0.041(5) 0.040(5) C4A 0.172(12) 0.107(8) 0.087(8) 0.066(7) 0.049(8) 0.090(8) C4B 0.103(7) 0.062(5) 0.064(5) 0.031(4) 0.023(5) 0.007(5) C5A 0.181(11) 0.110(8) 0.082(7) 0.057(7) 0.085(8) 0.095(9) C5B 0.064(4) 0.059(4) 0.058(4) 0.026(4) 0.010(3) 0.024(3) C6 0.050(3) 0.040(3) 0.033(3) 0.009(3) 0.002(3) 0.017(3) C6A 0.058(4) 0.049(4) 0.042(4) 0.018(3) 0.001(3) 0.003(3) C7 0.149(9) 0.074(6) 0.075(6) -0.002(5) 0.030(6) 0.031(6) C7A 0.052(4) 0.065(4) 0.049(4) 0.020(3) 0.004(3) 0.023(3) C8A 0.052(4) 0.059(4) 0.039(3) 0.023(3) 0.011(3) 0.024(3) C9 0.082(5) 0.102(6) 0.106(7) 0.047(5) 0.028(5) 0.063(5) C9A 0.066(5) 0.088(6) 0.053(5) 0.015(4) 0.017(4) 0.036(4) C10 0.077(6) 0.173(11) 0.138(9) 0.096(9) 0.025(6) 0.030(6) C10A 0.109(8) 0.068(6) 0.054(5) 0.017(5) -0.012(5) 0.009(5) C11 0.147(9) 0.070(6) 0.125(9) 0.021(6) 0.043(7) 0.050(6) F1 0.053(3) 0.163(5) 0.095(4) 0.014(3) 0.033(2) 0.037(3) F1B 0.103(4) 0.097(4) 0.139(5) 0.015(3) 0.085(4) 0.014(3) F2 0.104(4) 0.200(6) 0.046(3) 0.041(3) 0.036(2) 0.080(4) F2B 0.172(6) 0.151(5) 0.136(5) 0.073(4) 0.088(4) 0.124(5) F3 0.120(4) 0.087(4) 0.117(4) 0.002(3) 0.035(3) 0.058(3) F3B 0.118(4) 0.114(4) 0.060(3) 0.022(3) 0.023(3) 0.040(3) F4A 0.125(12) 0.110(13) 0.076(9) -0.038(8) 0.013(8) -0.017(10) F4C 0.323(10) 0.109(5) 0.061(4) 0.054(3) -0.006(5) 0.008(5) F4D 0.096(11) 0.048(7) 0.19(2) -0.003(9) -0.011(11) 0.022(7) F5A 0.22(2) 0.184(18) 0.114(11) 0.067(13) -0.043(13) -0.145(16) F5B 0.276(9) 0.090(4) 0.125(5) 0.070(4) 0.073(5) 0.076(5) F5D 0.027(9) 0.13(2) 0.15(3) 0.002(19) 0.021(11) 0.006(12) F6A 0.144(6) 0.158(7) 0.124(6) 0.049(6) -0.060(5) -0.010(6) F6C 0.132(6) 0.214(8) 0.308(11) 0.208(9) 0.084(6) 0.023(6) F7A 0.279(9) 0.164(6) 0.067(4) 0.047(4) 0.077(5) 0.147(7) F8 0.268(12) 0.55(3) 0.137(7) 0.157(12) 0.145(8) 0.257(16) F9A 0.241(18) 0.141(13) 0.055(7) -0.038(8) 0.065(10) -0.062(14) F9B 0.259(17) 0.072(7) 0.083(7) 0.046(6) 0.107(10) 0.117(10) F10A 0.444(16) 0.228(9) 0.157(7) 0.141(7) 0.144(9) 0.275(12) F11A 0.137(16) 0.20(2) 0.24(3) 0.14(2) -0.051(16) 0.053(14) F11B 0.23(3) 0.169(17) 0.056(8) 0.047(8) 0.009(11) 0.14(2) F12A 0.273(11) 0.279(12) 0.249(11) 0.229(11) 0.140(11) 0.172(11) Mn1 0.0531(8) 0.0871(11) 0.0536(8) 0.0451(8) 0.0242(6) 0.0438(7) Mn2 0.0568(6) 0.0462(5) 0.0334(5) 0.0177(4) 0.0169(4) 0.0255(4) N1 0.049(3) 0.050(3) 0.038(3) 0.023(2) 0.015(2) 0.025(2) N2 0.050(3) 0.049(3) 0.038(3) 0.020(2) 0.012(2) 0.024(2) N3 0.051(3) 0.050(3) 0.035(3) 0.021(2) 0.011(2) 0.023(2) O1 0.083(3) 0.125(4) 0.074(3) 0.060(3) 0.044(3) 0.071(3) O1A 0.077(3) 0.047(3) 0.046(3) 0.008(2) 0.014(2) 0.012(2) O1B 0.073(3) 0.091(4) 0.067(3) 0.050(3) 0.041(2) 0.053(3) O2 0.061(3) 0.067(3) 0.063(3) 0.040(2) 0.018(2) 0.018(2) O2A 0.050(3) 0.061(3) 0.039(2) 0.013(2) 0.0173(19) 0.018(2) O2B 0.086(3) 0.097(4) 0.066(3) 0.056(3) 0.040(3) 0.050(3) O3 0.078(3) 0.096(4) 0.063(3) 0.057(3) 0.040(2) 0.050(3) O3A 0.103(4) 0.072(3) 0.044(3) 0.025(2) 0.020(2) 0.053(3) O4 0.057(3) 0.061(3) 0.042(2) 0.014(2) 0.019(2) 0.018(2) O4A 0.092(3) 0.057(3) 0.047(2) 0.029(2) 0.037(2) 0.043(2) O5 0.048(2) 0.078(3) 0.068(3) 0.035(3) 0.019(2) 0.031(2) O6 0.059(3) 0.090(3) 0.063(3) 0.042(3) 0.010(2) 0.034(2) O7 0.077(3) 0.058(3) 0.070(3) 0.031(3) 0.015(3) 0.023(2) O8 0.086(3) 0.065(3) 0.051(3) 0.035(2) 0.023(2) 0.048(2) O9 0.093(4) 0.060(3) 0.073(4) -0.008(3) 0.001(3) 0.035(3) P1 0.0443(9) 0.0553(10) 0.0406(9) 0.0207(8) 0.0149(7) 0.0194(7) P2 0.0526(9) 0.0612(10) 0.0451(9) 0.0311(8) 0.0153(7) 0.0282(8) P3 0.0695(11) 0.0503(9) 0.0361(8) 0.0143(7) 0.0143(8) 0.0339(8) _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 C1 N1 1.331(7) . ? C1 N2 1.330(7) . ? C1 P1 1.825(5) . ? C1A O4A 1.254(7) . ? C1A C2A 1.370(9) . ? C1A C5A 1.526(11) . ? C1B O1B 1.233(8) . ? C1B C5B 1.382(9) . ? C1B C2B 1.541(9) . ? C2 N3 1.334(7) 2_676 ? C2 N1 1.344(7) . ? C2 P2 1.815(6) . ? C2A C3A 1.390(9) . ? C2A H2A 0.9300 . ? C2B F1B 1.293(8) . ? C2B F2B 1.303(9) . ? C2B F3B 1.308(9) . ? C3 O2 1.435(8) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3A O3A 1.225(7) . ? C3A C4A 1.534(11) . ? C3B C5B 1.393(9) . ? C3B O2B 1.246(8) . ? C3B C4B 1.516(10) . ? C4 O3 1.452(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4A F11B 1.23(2) . ? C4A F10A 1.257(11) . ? C4A F12A 1.344(14) . ? C4A F11A 1.31(2) . ? C4B F6C 1.266(10) . ? C4B F4C 1.275(9) . ? C4B F5B 1.292(10) . ? C5A F7A 1.249(11) . ? C5A F9B 1.243(13) . ? C5A F8 1.340(15) . ? C5A F9A 1.339(18) . ? C5B H5B 0.9300 . ? C6 N3 1.329(7) . ? C6 N2 1.347(7) 2_676 ? C6 P3 1.820(6) . ? C6A O1A 1.237(8) . ? C6A C7A 1.385(9) . ? C6A C10A 1.537(10) . ? C7 O9 1.378(9) . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7D 0.9600 . ? C7A C8A 1.373(9) . ? C7A H7A 0.9300 . ? C8A O2A 1.255(7) . ? C8A C9A 1.519(9) . ? C9 O5 1.434(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C9A F2 1.315(9) . ? C9A F1 1.318(8) . ? C9A F3 1.325(9) . ? C10 O1 1.378(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10A F5A 1.22(2) . ? C10A F6A 1.259(11) . ? C10A F4D 1.267(16) . ? C10A F5D 1.30(3) . ? C10A F4A 1.401(19) . ? C11 O7 1.449(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? F4A F4D 1.06(2) . ? F4D F5A 1.59(3) . ? F5A F5D 0.77(5) . ? F5D F6A 1.68(4) . ? F8 F9B 1.615(19) . ? F9A F9B 1.45(2) . ? F11A F11B 1.03(3) . ? Mn1 O2B 2.136(5) . ? Mn1 O2B 2.136(5) 2_777 ? Mn1 O1B 2.147(4) . ? Mn1 O1B 2.147(4) 2_777 ? Mn1 O6 2.167(4) . ? Mn1 O6 2.167(4) 2_777 ? Mn2 O4 2.148(4) . ? Mn2 O4A 2.168(4) . ? Mn2 O8 2.130(4) . ? Mn2 O2A 2.127(4) . ? Mn2 O3A 2.170(5) . ? Mn2 O1A 2.189(5) . ? N2 C6 1.347(7) 2_676 ? N3 C2 1.334(7) 2_676 ? O1 P3 1.528(5) . ? O2 P1 1.551(5) . ? O3 P2 1.543(4) . ? O4 P1 1.448(4) . ? O5 P1 1.550(4) . ? O6 P2 1.454(4) . ? O7 P2 1.554(5) . ? O8 P3 1.446(4) . ? O9 P3 1.545(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 125.7(5) . . ? N1 C1 P1 115.0(4) . . ? N2 C1 P1 119.3(4) . . ? O4A C1A C2A 129.0(6) . . ? O4A C1A C5A 113.9(6) . . ? C2A C1A C5A 117.1(7) . . ? O1B C1B C5B 129.6(6) . . ? O1B C1B C2B 112.5(6) . . ? C5B C1B C2B 117.9(6) . . ? N3 C2 N1 125.0(5) 2_676 . ? N3 C2 P2 121.6(4) 2_676 . ? N1 C2 P2 113.4(4) . . ? C1A C2A C3A 122.2(6) . . ? C1A C2A H2A 118.9 . . ? C3A C2A H2A 118.9 . . ? F1B C2B F2B 107.8(7) . . ? F1B C2B F3B 108.0(7) . . ? F2B C2B F3B 105.7(7) . . ? F1B C2B C1B 111.4(6) . . ? F2B C2B C1B 113.7(7) . . ? F3B C2B C1B 110.1(6) . . ? O2 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3A C3A C2A 128.4(6) . . ? O3A C3A C4A 114.8(7) . . ? C2A C3A C4A 116.8(7) . . ? C5B C3B O2B 129.0(6) . . ? C5B C3B C4B 117.2(7) . . ? O2B C3B C4B 113.9(7) . . ? O3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? F11B C4A F10A 124.8(13) . . ? F11B C4A F12A 82.6(15) . . ? F10A C4A F12A 103.0(11) . . ? F11B C4A F11A 47.7(14) . . ? F10A C4A F11A 93.9(16) . . ? F12A C4A F11A 126.7(17) . . ? F11B C4A C3A 114.3(12) . . ? F10A C4A C3A 115.8(9) . . ? F12A C4A C3A 107.3(10) . . ? F11A C4A C3A 109.8(14) . . ? F6C C4B F4C 108.9(9) . . ? F6C C4B F5B 102.3(8) . . ? F4C C4B F5B 106.4(9) . . ? F6C C4B C3B 111.0(8) . . ? F4C C4B C3B 110.9(7) . . ? F5B C4B C3B 116.8(7) . . ? F7A C5A F9B 125.7(10) . . ? F7A C5A F8 94.0(10) . . ? F9B C5A F8 77.3(11) . . ? F7A C5A F9A 87.0(14) . . ? F9B C5A F9A 68.1(13) . . ? F8 C5A F9A 137.4(13) . . ? F7A C5A C1A 116.9(8) . . ? F9B C5A C1A 116.8(9) . . ? F8 C5A C1A 107.9(11) . . ? F9A C5A C1A 109.4(9) . . ? C3B C5B C1B 122.3(6) . . ? C3B C5B H5B 118.9 . . ? C1B C5B H5B 118.9 . . ? N3 C6 N2 126.1(5) . 2_676 ? N3 C6 P3 117.9(4) . . ? N2 C6 P3 115.9(4) 2_676 . ? O1A C6A C7A 128.6(6) . . ? O1A C6A C10A 115.8(7) . . ? C7A C6A C10A 115.6(7) . . ? O9 C7 H7B 109.5 . . ? O9 C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O9 C7 H7D 109.5 . . ? H7B C7 H7D 109.5 . . ? H7C C7 H7D 109.5 . . ? C8A C7A C6A 122.2(6) . . ? C8A C7A H7A 118.9 . . ? C6A C7A H7A 118.9 . . ? O2A C8A C7A 129.4(6) . . ? O2A C8A C9A 112.2(5) . . ? C7A C8A C9A 118.3(6) . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F2 C9A F1 108.0(7) . . ? F2 C9A F3 105.6(7) . . ? F1 C9A F3 107.1(7) . . ? F2 C9A C8A 111.0(6) . . ? F1 C9A C8A 113.4(6) . . ? F3 C9A C8A 111.3(7) . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F5A C10A F6A 113.7(16) . . ? F5A C10A F4D 79.2(15) . . ? F6A C10A F4D 121.9(14) . . ? F5A C10A F5D 35(2) . . ? F6A C10A F5D 82(2) . . ? F4D C10A F5D 108(2) . . ? F5A C10A F4A 120.9(16) . . ? F6A C10A F4A 85.0(12) . . ? F4D C10A F4A 46.5(13) . . ? F5D C10A F4A 134.5(17) . . ? F5A C10A C6A 114.5(11) . . ? F6A C10A C6A 111.0(8) . . ? F4D C10A C6A 113.1(11) . . ? F5D C10A C6A 117.2(17) . . ? F4A C10A C6A 108.1(10) . . ? O7 C11 H11A 109.5 . . ? O7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? F4D F4A C10A 60.1(13) . . ? F4A F4D C10A 73.4(17) . . ? F4A F4D F5A 118(2) . . ? C10A F4D F5A 49.2(10) . . ? F5D F5A C10A 78(3) . . ? F5D F5A F4D 121(4) . . ? C10A F5A F4D 51.6(11) . . ? F5A F5D C10A 67(2) . . ? F5A F5D F6A 111(4) . . ? C10A F5D F6A 48.0(13) . . ? C10A F6A F5D 50.3(11) . . ? C5A F8 F9B 48.7(7) . . ? C5A F9A F9B 52.8(9) . . ? C5A F9B F9A 59.1(10) . . ? C5A F9B F8 54.0(9) . . ? F9A F9B F8 109.1(11) . . ? F11B F11A C4A 61.8(19) . . ? F11A F11B C4A 71(2) . . ? O2B Mn1 O2B 180.00 . . ? O2B Mn1 O1B 84.50(18) . . ? O2B Mn1 O1B 95.50(18) 2_777 . ? O2B Mn1 O1B 95.50(18) . 2_777 ? O2B Mn1 O1B 84.50(18) 2_777 2_777 ? O1B Mn1 O1B 180.0 . . ? O2B Mn1 O6 89.61(19) . . ? O2B Mn1 O6 90.39(19) 2_777 . ? O1B Mn1 O6 90.74(19) . . ? O1B Mn1 O6 89.26(19) 2_777 . ? O2B Mn1 O6 90.39(19) . 2_777 ? O2B Mn1 O6 89.61(19) 2_777 2_777 ? O1B Mn1 O6 89.26(19) . 2_777 ? O1B Mn1 O6 90.74(19) 2_777 2_777 ? O6 Mn1 O6 180.0 . . ? O4 Mn2 O4A 104.10(16) . . ? O4 Mn2 O8 90.44(18) . . ? O4A Mn2 O8 87.51(16) . . ? O4 Mn2 O2A 88.67(15) . . ? O4A Mn2 O2A 166.81(17) . . ? O8 Mn2 O2A 95.83(17) . . ? O4 Mn2 O3A 87.98(19) . . ? O4A Mn2 O3A 81.81(16) . . ? O8 Mn2 O3A 168.47(17) . . ? O2A Mn2 O3A 95.55(17) . . ? O4 Mn2 O1A 171.09(16) . . ? O4A Mn2 O1A 84.64(17) . . ? O8 Mn2 O1A 88.20(18) . . ? O2A Mn2 O1A 82.72(17) . . ? O3A Mn2 O1A 95.08(19) . . ? C1 N1 C2 114.9(5) . . ? C1 N2 C6 113.8(5) . 2_676 ? C6 N3 C2 114.4(5) . 2_676 ? C10 O1 P3 125.1(6) . . ? C6A O1A Mn2 125.7(4) . . ? C1B O1B Mn1 127.2(4) . . ? P1 O2 C3 125.7(5) . . ? C8A O2A Mn2 126.6(4) . . ? C3B O2B Mn1 127.4(4) . . ? C4 O3 P2 121.7(5) . . ? C3A O3A Mn2 127.8(4) . . ? P1 O4 Mn2 154.9(3) . . ? C1A O4A Mn2 125.6(4) . . ? C9 O5 P1 122.7(5) . . ? P2 O6 Mn1 150.2(3) . . ? C11 O7 P2 124.0(5) . . ? P3 O8 Mn2 153.2(3) . . ? C7 O9 P3 127.1(6) . . ? O2 P1 O5 104.9(3) . . ? O2 P1 O4 111.4(3) . . ? O5 P1 O4 116.4(3) . . ? O2 P1 C1 107.7(3) . . ? O5 P1 C1 103.8(2) . . ? O4 P1 C1 112.1(2) . . ? O7 P2 O6 113.7(3) . . ? O7 P2 O3 105.4(3) . . ? O6 P2 O3 116.6(3) . . ? O7 P2 C2 106.1(3) . . ? O6 P2 C2 111.0(3) . . ? O3 P2 C2 103.1(3) . . ? O1 P3 O9 106.1(3) . . ? O1 P3 O8 115.2(3) . . ? O9 P3 O8 116.2(3) . . ? O1 P3 C6 106.5(3) . . ? O9 P3 C6 99.2(3) . . ? O8 P3 C6 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.552 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.101