# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gabor Speier' _publ_contact_author_email SPEIER@ALMOS.VEIN.HU _publ_section_title ; ; loop_ _publ_author_name 'Gabor Speier' 'Gabor Barath' 'Jozsef Kaizer' 'Erno Kuzmann' 'Laszlo Parkanyi' 'Attila Vertes' # Attachment 'bg72.cif' data_bg72 _database_code_depnum_ccdc_archive 'CCDC 719842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H23 Fe N2 O5' _chemical_formula_sum 'C31 H23 Fe N2 O5' _chemical_formula_weight 559.36 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.505(9) _cell_length_b 12.060(11) _cell_length_c 13.489(12) _cell_angle_alpha 63.650(12) _cell_angle_beta 67.833(17) _cell_angle_gamma 85.29(2) _cell_volume 1411(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1450 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 25.42 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.680 _exptl_crystal_size_mid 0.550 _exptl_crystal_size_min 0.430 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Empirical Absorption Correction (T.Higashi,2001) ; _exptl_absorpt_correction_T_max 0.780 _exptl_absorpt_correction_T_min 0.280 _exptl_special_details ; The rather low quality crystals do not diffract beyond theta 20-22 deg. After the SQUEEZE procedure a 150 A3 solvent-accessible volume remains. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type RAXIS-RAPID _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12569 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 22.47 _reflns_number_total 3583 _reflns_number_gt 2536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'Flipper/PLATON (G.Oszlanyi, A.L.Spek, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.' _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^)+(0.0709P)^2^+2.7386P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3583 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 Fe1 Fe 0.25756(9) 0.14277(9) 0.74115(8) 0.0540(3) Uani 1 1 d . . . O1 O 0.2302(4) 0.2101(4) 0.8502(4) 0.0623(12) Uani 1 1 d . . . O1A O 0.3529(4) 0.0082(4) 0.8185(4) 0.0553(11) Uani 1 1 d . . . O2 O 0.2086(4) 0.2974(4) 0.6067(4) 0.0597(12) Uani 1 1 d . . . O3 O 0.4403(4) 0.2209(4) 0.6187(4) 0.0566(11) Uani 1 1 d . . . O4 O 0.5608(4) 0.5031(4) 0.3418(4) 0.0561(11) Uani 1 1 d . . . N1 N 0.0377(5) 0.1008(5) 0.8205(5) 0.0535(13) Uani 1 1 d . . . N1A N 0.2210(5) 0.0275(5) 0.6749(5) 0.0559(14) Uani 1 1 d . . . C1 C -0.0167(6) 0.0277(7) 0.7804(6) 0.0656(19) Uani 1 1 d . . . H1A H -0.1023 0.0574 0.7715 0.079 Uiso 1 1 calc R . . H1B H -0.0360 -0.0590 0.8393 0.079 Uiso 1 1 calc R . . C2 C -0.0466(7) 0.1390(6) 0.8925(6) 0.0594(18) Uani 1 1 d . . . H2 H -0.1400 0.1182 0.9154 0.071 Uiso 1 1 calc R . . C3 C -0.0135(7) 0.2104(6) 0.9419(6) 0.0590(17) Uani 1 1 d . . . C4 C -0.1208(7) 0.2468(7) 1.0178(7) 0.075(2) Uani 1 1 d . . . H4 H -0.2118 0.2273 1.0318 0.090 Uiso 1 1 calc R . . C5 C -0.0952(9) 0.3105(7) 1.0722(8) 0.092(3) Uani 1 1 d . . . H5 H -0.1682 0.3328 1.1231 0.110 Uiso 1 1 calc R . . C6 C 0.0380(9) 0.3409(7) 1.0509(7) 0.085(2) Uani 1 1 d . . . H6 H 0.0554 0.3857 1.0864 0.102 Uiso 1 1 calc R . . C7 C 0.1462(8) 0.3064(6) 0.9784(7) 0.072(2) Uani 1 1 d . . . H7 H 0.2360 0.3262 0.9669 0.086 Uiso 1 1 calc R . . C8 C 0.1240(7) 0.2411(6) 0.9204(6) 0.0575(17) Uani 1 1 d . . . C1A C 0.0885(7) 0.0396(7) 0.6616(6) 0.0680(19) Uani 1 1 d . . . H1AA H 0.0678 -0.0255 0.6446 0.082 Uiso 1 1 calc R . . H1BA H 0.0892 0.1197 0.5971 0.082 Uiso 1 1 calc R . . C2A C 0.2975(7) -0.0556(7) 0.6570(6) 0.0671(19) Uani 1 1 d . . . H2A H 0.2721 -0.1007 0.6253 0.081 Uiso 1 1 calc R . . C3A C 0.4190(7) -0.0827(7) 0.6828(6) 0.0657(19) Uani 1 1 d . . . C4A C 0.5135(8) -0.1499(7) 0.6320(7) 0.082(2) Uani 1 1 d . . . H4A H 0.4957 -0.1737 0.5812 0.099 Uiso 1 1 calc R . . C5A C 0.6285(9) -0.1809(8) 0.6542(8) 0.096(3) Uani 1 1 d . . . H5A H 0.6907 -0.2237 0.6176 0.115 Uiso 1 1 calc R . . C6A C 0.6548(8) -0.1484(8) 0.7334(8) 0.094(3) Uani 1 1 d . . . H6A H 0.7348 -0.1693 0.7490 0.113 Uiso 1 1 calc R . . C7A C 0.5606(8) -0.0848(7) 0.7880(7) 0.079(2) Uani 1 1 d . . . H7A H 0.5773 -0.0646 0.8413 0.094 Uiso 1 1 calc R . . C8A C 0.4422(7) -0.0512(6) 0.7641(6) 0.0593(18) Uani 1 1 d . . . C9 C 0.3158(6) 0.3656(6) 0.5201(6) 0.0498(16) Uani 1 1 d . . . C10 C 0.4465(6) 0.3253(6) 0.5244(6) 0.0517(16) Uani 1 1 d . . . C11 C 0.5658(6) 0.3935(6) 0.4341(6) 0.0523(16) Uani 1 1 d . . . C12 C 0.4386(7) 0.5448(6) 0.3369(6) 0.0541(16) Uani 1 1 d . . . C13 C 0.4433(7) 0.6583(6) 0.2445(6) 0.0654(19) Uani 1 1 d . . . H13 H 0.5278 0.7042 0.1892 0.078 Uiso 1 1 calc R . . C14 C 0.3220(8) 0.7039(7) 0.2338(7) 0.079(2) Uani 1 1 d . . . H14 H 0.3244 0.7810 0.1716 0.095 Uiso 1 1 calc R . . C15 C 0.1953(7) 0.6341(7) 0.3166(7) 0.077(2) Uani 1 1 d . . . H15 H 0.1138 0.6640 0.3079 0.092 Uiso 1 1 calc R . . C16 C 0.1907(7) 0.5240(6) 0.4089(6) 0.0609(18) Uani 1 1 d . . . H16 H 0.1059 0.4786 0.4640 0.073 Uiso 1 1 calc R . . C17 C 0.3124(6) 0.4773(6) 0.4226(5) 0.0501(15) Uani 1 1 d . . . C18 C 0.7055(6) 0.3632(6) 0.4188(6) 0.0520(16) Uani 1 1 d . . . C19 C 0.8161(6) 0.4486(6) 0.3242(6) 0.0632(18) Uani 1 1 d . . . H19 H 0.7986 0.5242 0.2718 0.076 Uiso 1 1 calc R . . C20 C 0.9506(7) 0.4225(8) 0.3074(7) 0.075(2) Uani 1 1 d . . . H20 H 1.0231 0.4816 0.2456 0.090 Uiso 1 1 calc R . . C21 C 0.9774(7) 0.3100(9) 0.3813(8) 0.079(2) Uani 1 1 d . . . H21 H 1.0684 0.2916 0.3681 0.094 Uiso 1 1 calc R . . C22 C 0.8704(7) 0.2231(7) 0.4759(7) 0.076(2) Uani 1 1 d . . . H22 H 0.8890 0.1469 0.5266 0.091 Uiso 1 1 calc R . . C23 C 0.7355(7) 0.2508(7) 0.4943(6) 0.0635(18) Uani 1 1 d . . . H23 H 0.6636 0.1929 0.5586 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0482(5) 0.0525(6) 0.0516(6) -0.0203(5) -0.0117(4) -0.0011(4) O1 0.053(3) 0.074(3) 0.065(3) -0.042(3) -0.015(2) 0.007(2) O1A 0.059(3) 0.052(3) 0.049(3) -0.020(2) -0.017(2) 0.007(2) O2 0.050(3) 0.052(3) 0.057(3) -0.015(2) -0.012(2) -0.001(2) O3 0.047(2) 0.052(3) 0.055(3) -0.014(2) -0.013(2) 0.000(2) O4 0.045(2) 0.055(3) 0.056(3) -0.018(2) -0.014(2) 0.004(2) N1 0.052(3) 0.049(3) 0.052(3) -0.016(3) -0.018(3) -0.002(3) N1A 0.051(3) 0.062(4) 0.059(4) -0.028(3) -0.025(3) 0.006(3) C1 0.052(4) 0.069(5) 0.070(5) -0.024(4) -0.024(4) -0.003(3) C2 0.047(4) 0.049(4) 0.054(4) -0.004(4) -0.012(3) 0.004(3) C3 0.061(4) 0.050(4) 0.050(4) -0.017(3) -0.009(4) -0.003(3) C4 0.062(4) 0.064(5) 0.071(5) -0.023(4) -0.004(4) 0.006(4) C5 0.094(7) 0.072(6) 0.085(6) -0.040(5) -0.004(5) 0.010(5) C6 0.091(6) 0.073(5) 0.081(6) -0.046(5) -0.007(5) -0.003(5) C7 0.074(5) 0.052(4) 0.082(5) -0.029(4) -0.021(4) -0.002(4) C8 0.064(4) 0.042(4) 0.052(4) -0.015(3) -0.012(4) -0.007(3) C1A 0.074(5) 0.069(5) 0.067(5) -0.027(4) -0.035(4) 0.003(4) C2A 0.067(5) 0.069(5) 0.060(5) -0.029(4) -0.016(4) -0.004(4) C3A 0.065(5) 0.069(5) 0.059(5) -0.030(4) -0.018(4) 0.007(4) C4A 0.077(5) 0.089(6) 0.089(6) -0.051(5) -0.028(5) 0.024(5) C5A 0.097(7) 0.110(7) 0.096(7) -0.067(6) -0.032(6) 0.037(6) C6A 0.073(5) 0.111(7) 0.109(7) -0.057(6) -0.040(5) 0.030(5) C7A 0.073(5) 0.095(6) 0.084(6) -0.048(5) -0.041(5) 0.034(4) C8A 0.056(4) 0.051(4) 0.046(4) -0.011(3) -0.007(3) 0.001(3) C9 0.044(4) 0.046(4) 0.049(4) -0.021(3) -0.006(3) -0.001(3) C10 0.046(4) 0.047(4) 0.050(4) -0.021(4) -0.005(3) -0.002(3) C11 0.052(4) 0.045(4) 0.055(4) -0.021(4) -0.016(3) 0.004(3) C17 0.053(4) 0.044(4) 0.048(4) -0.017(3) -0.018(3) 0.002(3) C12 0.063(4) 0.043(4) 0.056(4) -0.023(4) -0.021(4) 0.005(3) C13 0.060(4) 0.057(5) 0.070(5) -0.017(4) -0.028(4) 0.001(3) C14 0.090(6) 0.057(5) 0.074(5) -0.008(4) -0.040(5) 0.002(4) C15 0.058(4) 0.072(5) 0.085(6) -0.023(5) -0.026(4) 0.005(4) C16 0.052(4) 0.053(4) 0.066(5) -0.018(4) -0.021(4) 0.004(3) C18 0.040(3) 0.054(4) 0.053(4) -0.024(4) -0.007(3) -0.002(3) C19 0.052(4) 0.062(4) 0.067(5) -0.027(4) -0.014(4) -0.001(3) C20 0.044(4) 0.088(6) 0.086(6) -0.046(5) -0.007(4) -0.007(4) C21 0.046(4) 0.102(7) 0.090(6) -0.053(6) -0.017(4) 0.014(5) C22 0.065(5) 0.081(5) 0.090(6) -0.042(5) -0.035(5) 0.019(4) C23 0.050(4) 0.066(5) 0.068(5) -0.027(4) -0.020(4) 0.010(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 Fe1 O1 1.899(4) . ? Fe1 O1A 1.935(4) . ? Fe1 O3 1.955(4) . ? Fe1 N1A 2.080(5) . ? Fe1 O2 2.139(4) . ? Fe1 N1 2.141(5) . ? O2 C9 1.272(7) . ? O1 C8 1.316(7) . ? O1A C8A 1.330(7) . ? O3 C10 1.318(7) . ? O4 C12 1.354(7) . ? O4 C11 1.370(7) . ? N1 C2 1.273(8) . ? N1 C1 1.462(8) . ? N1A C2A 1.283(8) . ? N1A C1A 1.457(8) . ? C1 C1A 1.515(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.428(9) . ? C2 H2 0.9300 . ? C3 C4 1.399(9) . ? C3 C8 1.408(9) . ? C4 C5 1.372(10) . ? C4 H4 0.9300 . ? C5 C6 1.366(11) . ? C5 H5 0.9300 . ? C6 C7 1.367(10) . ? C6 H6 0.9300 . ? C7 C8 1.415(9) . ? C7 H7 0.9300 . ? C1A H1AA 0.9700 . ? C1A H1BA 0.9700 . ? C2A C3A 1.423(10) . ? C2A H2A 0.9300 . ? C3A C4A 1.400(9) . ? C3A C8A 1.412(9) . ? C4A C5A 1.337(11) . ? C4A H4A 0.9300 . ? C5A C6A 1.409(11) . ? C5A H5A 0.9300 . ? C6A C7A 1.393(10) . ? C6A H6A 0.9300 . ? C7A C8A 1.385(9) . ? C7A H7A 0.9300 . ? C9 C17 1.414(8) . ? C9 C10 1.432(8) . ? C10 C11 1.363(8) . ? C11 C18 1.442(8) . ? C17 C12 1.394(8) . ? C17 C16 1.398(8) . ? C12 C13 1.371(9) . ? C13 C14 1.379(9) . ? C13 H13 0.9300 . ? C14 C15 1.397(10) . ? C14 H14 0.9300 . ? C15 C16 1.347(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C23 1.386(9) . ? C18 C19 1.396(8) . ? C19 C20 1.377(9) . ? C19 H19 0.9300 . ? C20 C21 1.366(10) . ? C20 H20 0.9300 . ? C21 C22 1.384(10) . ? C21 H21 0.9300 . ? C22 C23 1.382(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O1A 93.21(19) . . ? O1 Fe1 O3 103.14(19) . . ? O1A Fe1 O3 86.23(18) . . ? O1 Fe1 N1A 158.29(19) . . ? O1A Fe1 N1A 84.5(2) . . ? O3 Fe1 N1A 98.26(19) . . ? O1 Fe1 O2 98.6(2) . . ? O1A Fe1 O2 161.72(16) . . ? O3 Fe1 O2 77.56(17) . . ? N1A Fe1 O2 89.5(2) . . ? O1 Fe1 N1 85.18(19) . . ? O1A Fe1 N1 113.00(19) . . ? O3 Fe1 N1 158.85(19) . . ? N1A Fe1 N1 76.0(2) . . ? O2 Fe1 N1 82.01(18) . . ? C9 O2 Fe1 112.4(4) . . ? C8 O1 Fe1 136.0(4) . . ? C8A O1A Fe1 124.1(4) . . ? C10 O3 Fe1 117.8(4) . . ? C12 O4 C11 121.2(5) . . ? C2 N1 C1 119.1(5) . . ? C2 N1 Fe1 125.8(4) . . ? C1 N1 Fe1 115.0(4) . . ? C2A N1A C1A 120.9(6) . . ? C2A N1A Fe1 125.6(5) . . ? C1A N1A Fe1 113.2(4) . . ? N1 C1 C1A 109.4(5) . . ? N1 C1 H1A 109.8 . . ? C1A C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C1A C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C3 127.2(6) . . ? N1 C2 H2 116.4 . . ? C3 C2 H2 116.4 . . ? C4 C3 C8 118.9(7) . . ? C4 C3 C2 119.1(6) . . ? C8 C3 C2 121.9(6) . . ? C5 C4 C3 121.6(7) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 119.6(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.9(8) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C8 121.1(7) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? O1 C8 C3 122.4(6) . . ? O1 C8 C7 119.8(6) . . ? C3 C8 C7 117.8(6) . . ? N1A C1A C1 105.3(5) . . ? N1A C1A H1AA 110.7 . . ? C1 C1A H1AA 110.7 . . ? N1A C1A H1BA 110.7 . . ? C1 C1A H1BA 110.7 . . ? H1AA C1A H1BA 108.8 . . ? N1A C2A C3A 123.6(7) . . ? N1A C2A H2A 118.2 . . ? C3A C2A H2A 118.2 . . ? C4A C3A C8A 119.2(7) . . ? C4A C3A C2A 118.7(7) . . ? C8A C3A C2A 122.0(6) . . ? C5A C4A C3A 122.0(8) . . ? C5A C4A H4A 119.0 . . ? C3A C4A H4A 119.0 . . ? C4A C5A C6A 119.6(8) . . ? C4A C5A H5A 120.2 . . ? C6A C5A H5A 120.2 . . ? C7A C6A C5A 119.6(8) . . ? C7A C6A H6A 120.2 . . ? C5A C6A H6A 120.2 . . ? C8A C7A C6A 120.9(7) . . ? C8A C7A H7A 119.5 . . ? C6A C7A H7A 119.5 . . ? O1A C8A C7A 119.8(6) . . ? O1A C8A C3A 121.6(6) . . ? C7A C8A C3A 118.6(6) . . ? O2 C9 C17 124.0(6) . . ? O2 C9 C10 116.8(6) . . ? C17 C9 C10 119.3(6) . . ? O3 C10 C11 124.8(6) . . ? O3 C10 C9 115.3(5) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 O4 120.1(6) . . ? C10 C11 C18 127.7(6) . . ? O4 C11 C18 112.2(5) . . ? C12 C17 C16 118.8(6) . . ? C12 C17 C9 117.3(6) . . ? C16 C17 C9 123.9(6) . . ? O4 C12 C13 117.3(6) . . ? O4 C12 C17 122.0(6) . . ? C13 C12 C17 120.7(6) . . ? C12 C13 C14 119.6(7) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.4(7) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.5(6) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C23 C18 C19 117.9(6) . . ? C23 C18 C11 122.5(6) . . ? C19 C18 C11 119.7(6) . . ? C20 C19 C18 121.1(7) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.0(7) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.5(7) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.4(7) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C18 121.2(7) . . ? C22 C23 H23 119.4 . . ? C18 C23 H23 119.4 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 22.47 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.263 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.063 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 149 8 ' ' 2 0.500 0.000 0.000 33 13 ' ' _platon_squeeze_details ; ;