# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Banglin Chen' _publ_contact_author_email Banglin.Chen@utsa.edu loop_ _publ_author_name 'Yabing He' 'Banglin Chen' # Attachment '- UTSA-30.CIF' data_156 _database_code_depnum_ccdc_archive 'CCDC 894905' #TrackingRef '- UTSA-30.CIF' _vrf_CHEMW03_156 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1019.96 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 39.00 468.43 H 1.01 21.00 21.17 O 16.00 6.00 95.99 Yb 173.04 1.00 173.04 N 14.01 0.00 0.00 Calculated formula weight 758.63 RESPONSE: The SQUEEZE routine from within PLATON was used to account for residual electron density that could not be reliably modeled. The electron count and void volume is close to a half N,N'-dimethylacetamide molecules from which the compound was crystallized. The atoms count for these solvents have been included to correctly represent formual weight, F(000), density, etc. SQUEEZE details can be found at the end of the CIF. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Yb(C39H21O6) (C4H9NO)3' _chemical_formula_sum 'C51 H48 N3 O9 Yb' _chemical_formula_weight 1019.96 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3m1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' '-x, -x+y, -z' 'x-y, -y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' 'x, x-y, z' '-x+y, y, z' _cell_length_a 17.0600(17) _cell_length_b 17.0600(17) _cell_length_c 9.2376(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2328.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_absorpt_coefficient_mu 2.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5952 _exptl_absorpt_correction_T_max 0.8045 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8212 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 30.46 _reflns_number_total 2457 _reflns_number_gt 1634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Shelx restraints used: SADI C15 c14 C15 c16 c13 c14 ISOR 0.2 0.4 C15 ISOR restraint was applied to the 'split' Cl5 atom from the naphthalene group. SADI restraint is applied to keep same C-C distance for the naphthalene group. ; _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^)+(0.1105P)^2^+4.5640P] 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 2457 _refine_ls_number_parameters 119 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _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 Yb1 Yb 0.0000 0.0000 0.5000 0.01175(19) Uani 1 12 d S . . Yb2 Yb 0.0000 0.0000 0.0000 0.01238(19) Uani 1 12 d S . . O1 O 0.06207(16) 0.1241(3) 0.3698(5) 0.0277(12) Uani 1 2 d S . . O2 O 0.06173(15) 0.1235(3) 0.1320(5) 0.0230(10) Uani 1 2 d S . . C11 C 0.0823(2) 0.1646(4) 0.2498(7) 0.0176(13) Uani 1 2 d S . . C12 C 0.1323(2) 0.2645(4) 0.2496(7) 0.0204(13) Uani 1 2 d S . 1 C13 C 0.1844(5) 0.3203(5) 0.1319(8) 0.0124(17) Uani 0.50 1 d PD . 1 C14 C 0.2137(6) 0.2900(7) 0.0266(10) 0.027(2) Uani 0.50 1 d PD . 1 H14A H 0.1973 0.2282 0.0183 0.032 Uiso 0.50 1 calc PR . 1 C15 C 0.2670(14) 0.3514(8) -0.066(2) 0.172(16) Uani 0.50 1 d PDU A 1 H15A H 0.2847 0.3276 -0.1440 0.206 Uiso 0.50 1 calc PR A 1 C16 C 0.3020(7) 0.4415(6) -0.0726(10) 0.0207(19) Uani 0.50 1 d PD A 1 H16A H 0.3451 0.4790 -0.1430 0.025 Uiso 0.50 1 calc PR A 1 C17 C 0.2688(6) 0.4734(6) 0.0329(10) 0.0209(19) Uani 0.50 1 d P . 1 C18 C 0.2083(2) 0.4165(5) 0.1389(6) 0.0208(14) Uani 1 2 d S . 1 C19 C 0.1840(6) 0.4481(7) 0.2525(11) 0.026(2) Uani 0.50 1 d P . 1 H19A H 0.2014 0.5109 0.2469 0.031 Uiso 0.50 1 d PR . 1 C20 C 0.1267(10) 0.3924(8) 0.3671(12) 0.039(3) Uani 0.50 1 d P B 1 H20A H 0.1072 0.4172 0.4414 0.047 Uiso 0.50 1 calc PR B 1 C21 C 0.1005(7) 0.3014(6) 0.3667(10) 0.0223(19) Uani 0.50 1 d P . 1 H21A H 0.0596 0.2609 0.4384 0.027 Uiso 0.50 1 d PR . 1 C22 C 0.2867(3) 0.5734(5) 0.0284(8) 0.043(2) Uani 1 2 d S . . C23 C 0.2397(5) 0.6198(3) 0.0272(8) 0.041(2) Uani 1 2 d S . . H23A H 0.1754 0.5877 0.0256 0.049 Uiso 1 2 calc SR . . 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 Yb1 0.0122(2) 0.0122(2) 0.0107(3) 0.000 0.000 0.00612(12) Yb2 0.0118(2) 0.0118(2) 0.0136(3) 0.000 0.000 0.00589(12) O1 0.038(2) 0.015(2) 0.022(2) 0.004(2) 0.0022(10) 0.0075(12) O2 0.031(2) 0.011(2) 0.020(2) -0.0051(18) -0.0026(9) 0.0057(11) C11 0.021(2) 0.008(3) 0.020(3) -0.001(2) -0.0005(12) 0.0039(14) C12 0.026(3) 0.009(3) 0.020(3) -0.002(2) -0.0012(12) 0.0046(14) C13 0.015(4) 0.009(3) 0.008(3) -0.001(3) -0.001(3) 0.002(3) C14 0.019(5) 0.018(5) 0.033(5) 0.007(4) -0.004(4) 0.002(4) C15 0.23(3) 0.038(10) 0.22(3) -0.039(15) -0.20(3) 0.049(15) C16 0.026(5) 0.015(4) 0.021(4) 0.003(4) 0.007(4) 0.010(4) C17 0.023(5) 0.011(4) 0.024(4) 0.001(3) -0.003(4) 0.005(4) C18 0.026(3) 0.022(3) 0.013(3) -0.006(3) -0.0032(13) 0.0110(17) C19 0.017(5) 0.025(5) 0.036(5) -0.002(4) -0.001(4) 0.009(4) C20 0.059(9) 0.027(6) 0.027(5) -0.004(5) 0.002(6) 0.019(6) C21 0.027(5) 0.016(4) 0.021(4) -0.001(4) -0.002(4) 0.009(4) C22 0.076(6) 0.013(4) 0.020(3) 0.000(3) -0.0001(14) 0.0064(18) C23 0.011(3) 0.068(5) 0.024(4) -0.0010(14) -0.002(3) 0.0057(17) _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 Yb1 O1 2.193(5) 2 ? Yb1 O1 2.193(5) 3 ? Yb1 O1 2.193(5) 8_556 ? Yb1 O1 2.193(5) 9_556 ? Yb1 O1 2.193(5) . ? Yb1 O1 2.193(5) 7_556 ? Yb2 O2 2.194(4) . ? Yb2 O2 2.194(4) 7 ? Yb2 O2 2.194(4) 9 ? Yb2 O2 2.194(4) 3 ? Yb2 O2 2.194(4) 8 ? Yb2 O2 2.194(4) 2 ? O1 C11 1.260(7) . ? O2 C11 1.247(7) . ? C11 C12 1.476(9) . ? C12 C13 1.425(9) 12 ? C12 C13 1.425(9) . ? C12 C21 1.483(11) 12 ? C12 C21 1.483(11) . ? C13 C13 0.827(15) 12 ? C13 C14 1.312(11) . ? C13 C18 1.482(10) . ? C13 C14 1.912(12) 12 ? C14 C15 1.303(16) . ? C14 C13 1.912(12) 12 ? C14 H14A 0.9500 . ? C15 C16 1.343(13) . ? C15 H15A 0.9500 . ? C16 C17 1.370(13) . ? C16 H16A 0.9500 . ? C17 C17 1.095(19) 12 ? C17 C18 1.401(11) . ? C17 C22 1.576(12) . ? C18 C19 1.336(11) 12 ? C18 C19 1.336(11) . ? C18 C17 1.401(11) 12 ? C18 C13 1.482(10) 12 ? C19 C19 1.366(19) 12 ? C19 C20 1.432(15) . ? C19 H19A 0.9600 . ? C20 C21 1.384(15) . ? C20 H20A 0.9500 . ? C21 C21 1.71(2) 12 ? C21 H21A 0.9598 . ? C22 C23 1.381(5) 2_665 ? C22 C23 1.381(5) . ? C22 C17 1.576(12) 12 ? C23 C22 1.381(5) 3_565 ? C23 H23A 0.9500 . ? 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 Yb1 O1 92.81(17) 2 3 ? O1 Yb1 O1 180.0(3) 2 8_556 ? O1 Yb1 O1 87.19(17) 3 8_556 ? O1 Yb1 O1 87.19(17) 2 9_556 ? O1 Yb1 O1 180.0 3 9_556 ? O1 Yb1 O1 92.81(17) 8_556 9_556 ? O1 Yb1 O1 92.81(17) 2 . ? O1 Yb1 O1 92.81(17) 3 . ? O1 Yb1 O1 87.19(17) 8_556 . ? O1 Yb1 O1 87.19(17) 9_556 . ? O1 Yb1 O1 87.19(17) 2 7_556 ? O1 Yb1 O1 87.19(17) 3 7_556 ? O1 Yb1 O1 92.81(17) 8_556 7_556 ? O1 Yb1 O1 92.81(17) 9_556 7_556 ? O1 Yb1 O1 180.0(2) . 7_556 ? O2 Yb2 O2 180.0(3) . 7 ? O2 Yb2 O2 87.90(16) . 9 ? O2 Yb2 O2 92.10(16) 7 9 ? O2 Yb2 O2 92.10(16) . 3 ? O2 Yb2 O2 87.90(16) 7 3 ? O2 Yb2 O2 180.0(3) 9 3 ? O2 Yb2 O2 87.90(16) . 8 ? O2 Yb2 O2 92.10(16) 7 8 ? O2 Yb2 O2 92.10(16) 9 8 ? O2 Yb2 O2 87.90(16) 3 8 ? O2 Yb2 O2 92.10(16) . 2 ? O2 Yb2 O2 87.90(16) 7 2 ? O2 Yb2 O2 87.90(16) 9 2 ? O2 Yb2 O2 92.10(16) 3 2 ? O2 Yb2 O2 180.0(3) 8 2 ? C11 O1 Yb1 151.6(4) . . ? C11 O2 Yb2 153.0(4) . . ? O2 C11 O1 122.5(6) . . ? O2 C11 C12 119.1(6) . . ? O1 C11 C12 118.4(6) . . ? C13 C12 C13 33.7(6) 12 . ? C13 C12 C11 125.4(6) 12 . ? C13 C12 C11 125.4(6) . . ? C13 C12 C21 120.7(6) 12 12 ? C13 C12 C21 100.2(5) . 12 ? C11 C12 C21 111.5(6) . 12 ? C13 C12 C21 100.2(5) 12 . ? C13 C12 C21 120.7(6) . . ? C11 C12 C21 111.5(6) . . ? C21 C12 C21 70.6(8) 12 . ? C13 C13 C14 125.3(5) 12 . ? C13 C13 C12 73.1(3) 12 . ? C14 C13 C12 122.4(8) . . ? C13 C13 C18 73.8(3) 12 . ? C14 C13 C18 121.4(7) . . ? C12 C13 C18 116.2(6) . . ? C13 C13 C14 34.1(3) 12 12 ? C14 C13 C14 91.2(8) . 12 ? C12 C13 C14 90.7(5) . 12 ? C18 C13 C14 90.9(5) . 12 ? C15 C14 C13 114.8(13) . . ? C15 C14 C13 114.5(13) . 12 ? C13 C14 C13 20.7(4) . 12 ? C15 C14 H14A 122.6 . . ? C13 C14 H14A 122.6 . . ? C13 C14 H14A 118.9 12 . ? C14 C15 C16 133(2) . . ? C14 C15 H15A 113.4 . . ? C16 C15 H15A 113.4 . . ? C15 C16 C17 112.6(14) . . ? C15 C16 H16A 123.7 . . ? C17 C16 H16A 123.7 . . ? C17 C17 C16 127.8(6) 12 . ? C17 C17 C18 67.0(4) 12 . ? C16 C17 C18 122.0(8) . . ? C17 C17 C22 69.7(4) 12 . ? C16 C17 C22 121.1(8) . . ? C18 C17 C22 116.4(7) . . ? C19 C18 C19 61.5(9) 12 . ? C19 C18 C17 122.6(8) 12 12 ? C19 C18 C17 98.0(7) . 12 ? C19 C18 C17 98.0(7) 12 . ? C19 C18 C17 122.6(8) . . ? C17 C18 C17 46.0(8) 12 . ? C19 C18 C13 120.7(7) 12 12 ? C19 C18 C13 103.1(6) . 12 ? C17 C18 C13 115.9(6) 12 12 ? C17 C18 C13 130.8(6) . 12 ? C19 C18 C13 103.1(6) 12 . ? C19 C18 C13 120.7(7) . . ? C17 C18 C13 130.8(6) 12 . ? C17 C18 C13 115.9(6) . . ? C13 C18 C13 32.4(6) 12 . ? C18 C19 C19 59.3(4) . 12 ? C18 C19 C20 124.0(10) . . ? C19 C19 C20 110.5(7) 12 . ? C18 C19 H19A 115.0 . . ? C19 C19 H19A 104.4 12 . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 118.2(11) . . ? C21 C20 H20A 120.9 . . ? C19 C20 H20A 120.9 . . ? C20 C21 C12 119.7(9) . . ? C20 C21 C21 103.7(7) . 12 ? C12 C21 C21 54.7(4) . 12 ? C20 C21 H21A 121.1 . . ? C12 C21 H21A 119.1 . . ? C21 C21 H21A 111.5 12 . ? C23 C22 C23 120.4(8) 2_665 . ? C23 C22 C17 140.1(6) 2_665 12 ? C23 C22 C17 99.5(5) . 12 ? C23 C22 C17 99.5(5) 2_665 . ? C23 C22 C17 140.1(6) . . ? C17 C22 C17 40.6(7) 12 . ? C22 C23 C22 119.6(8) 3_565 . ? C22 C23 H23A 120.2 3_565 . ? C22 C23 H23A 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Yb1 O1 C11 -46.48(10) 2 . . . ? O1 Yb1 O1 C11 46.48(9) 3 . . . ? O1 Yb1 O1 C11 133.52(10) 8_556 . . . ? O1 Yb1 O1 C11 -133.52(9) 9_556 . . . ? O1 Yb1 O1 C11 109(85) 7_556 . . . ? O2 Yb2 O2 C11 -73(85) 7 . . . ? O2 Yb2 O2 C11 133.91(9) 9 . . . ? O2 Yb2 O2 C11 -46.09(9) 3 . . . ? O2 Yb2 O2 C11 -133.91(9) 8 . . . ? O2 Yb2 O2 C11 46.09(9) 2 . . . ? Yb2 O2 C11 O1 0.000(3) . . . . ? Yb2 O2 C11 C12 180.000(3) . . . . ? Yb1 O1 C11 O2 0.000(3) . . . . ? Yb1 O1 C11 C12 180.000(3) . . . . ? O2 C11 C12 C13 20.8(4) . . . 12 ? O1 C11 C12 C13 -159.2(4) . . . 12 ? O2 C11 C12 C13 -20.8(4) . . . . ? O1 C11 C12 C13 159.2(4) . . . . ? O2 C11 C12 C21 -141.6(5) . . . 12 ? O1 C11 C12 C21 38.4(5) . . . 12 ? O2 C11 C12 C21 141.6(5) . . . . ? O1 C11 C12 C21 -38.4(5) . . . . ? C11 C12 C13 C13 102.4(4) . . . 12 ? C21 C12 C13 C13 -131.9(5) 12 . . 12 ? C21 C12 C13 C13 -58.5(5) . . . 12 ? C13 C12 C13 C14 -121.5(7) 12 . . . ? C11 C12 C13 C14 -19.1(10) . . . . ? C21 C12 C13 C14 106.6(9) 12 . . . ? C21 C12 C13 C14 180.0(8) . . . . ? C13 C12 C13 C18 61.7(6) 12 . . . ? C11 C12 C13 C18 164.2(3) . . . . ? C21 C12 C13 C18 -70.1(7) 12 . . . ? C21 C12 C13 C18 3.2(9) . . . . ? C13 C12 C13 C14 -29.6(4) 12 . . 12 ? C11 C12 C13 C14 72.8(5) . . . 12 ? C21 C12 C13 C14 -161.5(6) 12 . . 12 ? C21 C12 C13 C14 -88.1(6) . . . 12 ? C13 C13 C14 C15 94.2(12) 12 . . . ? C12 C13 C14 C15 -174.2(11) . . . . ? C18 C13 C14 C15 2.4(15) . . . . ? C14 C13 C14 C15 94.2(12) 12 . . . ? C12 C13 C14 C13 91.6(8) . . . 12 ? C18 C13 C14 C13 -91.8(7) . . . 12 ? C14 C13 C14 C13 0.000(3) 12 . . 12 ? C13 C14 C15 C16 3(3) . . . . ? C13 C14 C15 C16 26(2) 12 . . . ? C14 C15 C16 C17 -6(3) . . . . ? C15 C16 C17 C17 -81.4(12) . . . 12 ? C15 C16 C17 C18 2.9(15) . . . . ? C15 C16 C17 C22 -168.8(11) . . . . ? C17 C17 C18 C19 -128.4(6) 12 . . 12 ? C16 C17 C18 C19 110.3(10) . . . 12 ? C22 C17 C18 C19 -77.6(8) . . . 12 ? C17 C17 C18 C19 -67.2(6) 12 . . . ? C16 C17 C18 C19 171.5(8) . . . . ? C22 C17 C18 C19 -16.4(10) . . . . ? C16 C17 C18 C17 -121.3(8) . . . 12 ? C22 C17 C18 C17 50.8(7) . . . 12 ? C17 C17 C18 C13 88.1(6) 12 . . 12 ? C16 C17 C18 C13 -33.2(12) . . . 12 ? C22 C17 C18 C13 138.9(6) . . . 12 ? C17 C17 C18 C13 122.8(5) 12 . . . ? C16 C17 C18 C13 1.6(11) . . . . ? C22 C17 C18 C13 173.6(6) . . . . ? C13 C13 C18 C19 127.9(6) 12 . . 12 ? C14 C13 C18 C19 -110.3(9) . . . 12 ? C12 C13 C18 C19 66.5(7) . . . 12 ? C14 C13 C18 C19 157.7(6) 12 . . 12 ? C13 C13 C18 C19 63.5(5) 12 . . . ? C14 C13 C18 C19 -174.7(8) . . . . ? C12 C13 C18 C19 2.1(9) . . . . ? C14 C13 C18 C19 93.3(7) 12 . . . ? C13 C13 C18 C17 -73.3(6) 12 . . 12 ? C14 C13 C18 C17 48.5(11) . . . 12 ? C12 C13 C18 C17 -134.7(7) . . . 12 ? C14 C13 C18 C17 -43.5(8) 12 . . 12 ? C13 C13 C18 C17 -126.4(5) 12 . . . ? C14 C13 C18 C17 -4.5(10) . . . . ? C12 C13 C18 C17 172.3(6) . . . . ? C14 C13 C18 C17 -96.5(6) 12 . . . ? C14 C13 C18 C13 121.8(7) . . . 12 ? C12 C13 C18 C13 -61.4(6) . . . 12 ? C14 C13 C18 C13 29.9(4) 12 . . 12 ? C17 C18 C19 C19 -122.9(6) 12 . . 12 ? C17 C18 C19 C19 -80.9(6) . . . 12 ? C13 C18 C19 C19 118.1(6) 12 . . 12 ? C13 C18 C19 C19 88.6(6) . . . 12 ? C19 C18 C19 C20 -95.2(10) 12 . . . ? C17 C18 C19 C20 141.9(10) 12 . . . ? C17 C18 C19 C20 -176.1(9) . . . . ? C13 C18 C19 C20 22.9(11) 12 . . . ? C13 C18 C19 C20 -6.6(13) . . . . ? C18 C19 C20 C21 5.3(17) . . . . ? C19 C19 C20 C21 -60.7(12) 12 . . . ? C19 C20 C21 C12 0.3(16) . . . . ? C19 C20 C21 C21 57.3(11) . . . 12 ? C13 C12 C21 C20 -33.1(11) 12 . . . ? C13 C12 C21 C20 -4.4(12) . . . . ? C11 C12 C21 C20 -167.8(9) . . . . ? C21 C12 C21 C20 86.0(10) 12 . . . ? C13 C12 C21 C21 -119.2(6) 12 . . 12 ? C13 C12 C21 C21 -90.4(6) . . . 12 ? C11 C12 C21 C21 106.2(5) . . . 12 ? C17 C17 C22 C23 179.6(6) 12 . . 2_665 ? C16 C17 C22 C23 -57.7(10) . . . 2_665 ? C18 C17 C22 C23 130.1(7) . . . 2_665 ? C17 C17 C22 C23 0.6(10) 12 . . . ? C16 C17 C22 C23 123.2(12) . . . . ? C18 C17 C22 C23 -49.0(14) . . . . ? C16 C17 C22 C17 122.6(8) . . . 12 ? C18 C17 C22 C17 -49.5(7) . . . 12 ? C23 C22 C23 C22 -1.6(16) 2_665 . . 3_565 ? C17 C22 C23 C22 177.8(6) 12 . . 3_565 ? C17 C22 C23 C22 177.4(6) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 2.067 _refine_diff_density_min -1.390 _refine_diff_density_rms 0.197 # 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 0.029 0.514 -0.036 639 322 ' ' 2 0.289 0.144 0.299 29 19 ' ' 3 0.855 0.144 0.299 29 19 ' ' 4 0.856 0.711 0.299 29 19 ' ' 5 0.144 0.289 0.700 29 11 ' ' 6 0.144 0.855 0.700 29 10 ' ' 7 0.711 0.856 0.701 29 11 ' ' _platon_squeeze_details ; The electron density removed by the SQUEEZE process was estimated to correspond with three dimethyl acetamide molecules per formula unit. ;