############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,1-Diethyl-3-(4-methoxybenzoyl)thiourea ; _chemical_name_common ? _chemical_formula_moiety 'C13 H18 N2 O2 S' _chemical_formula_sum 'C13 H18 N2 O2 S' _chemical_formula_iupac 'C13 H18 N2 O2 S' _chemical_formula_weight 266.35 _chemical_melting_point_gt 407.15 _chemical_melting_point_lt 408.15 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 12.9024(5) _cell_length_b 10.0095(4) _cell_length_c 20.8585(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2693.8(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 5648 _cell_measurement_theta_min 4.24 _cell_measurement_theta_max 71.13 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 2.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2006) ; _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.900 _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1 K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _diffrn_ambient_temperature 150 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_device 'Oxford Diffraction Gemini' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12046 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 71.13 _diffrn_reflns_theta_full 71.13 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _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^ > \s(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. ; _reflns_number_total 2548 _reflns_number_gt 2214 _reflns_threshold_expression I>2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_gt 0.1165 _refine_ls_wR_factor_ref 0.1323 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_number_reflns 2548 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+0.6035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.427 _refine_diff_density_min -0.324 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELXTL (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.96773(4) 0.08865(5) 0.60731(2) 0.0302(2) Uani d . 1 1 . . O O1 0.72174(10) 0.27396(13) 0.63046(7) 0.0282(3) Uani d . 1 1 . . O O2 0.29590(10) 0.00839(15) 0.54492(7) 0.0327(4) Uani d . 1 1 . . N N1 0.76759(11) 0.05775(15) 0.63691(7) 0.0210(3) Uani d . 1 1 . . H H1A 0.7495 -0.0246 0.6332 0.025 Uiso calc R 1 1 . . N N2 0.87609(11) 0.11414(15) 0.72156(7) 0.0215(3) Uani d . 1 1 . . C C1 0.52575(14) 0.21406(19) 0.58056(9) 0.0242(4) Uani d . 1 1 . . H H1B 0.5472 0.3028 0.5811 0.029 Uiso calc R 1 1 . . C C2 0.42448(15) 0.1834(2) 0.56253(9) 0.0271(4) Uani d . 1 1 . . H H2A 0.3785 0.2510 0.5513 0.033 Uiso calc R 1 1 . . C C3 0.39293(14) 0.0509(2) 0.56149(8) 0.0246(4) Uani d . 1 1 . . C C4 0.46228(14) -0.05050(19) 0.57806(9) 0.0236(4) Uani d . 1 1 . . H H4A 0.4410 -0.1393 0.5771 0.028 Uiso calc R 1 1 . . C C5 0.56228(14) -0.01898(19) 0.59584(8) 0.0220(4) Uani d . 1 1 . . H H5A 0.6082 -0.0870 0.6067 0.026 Uiso calc R 1 1 . . C C6 0.59545(14) 0.11370(18) 0.59775(8) 0.0201(4) Uani d . 1 1 . . C C7 0.69945(13) 0.15522(17) 0.62164(8) 0.0202(4) Uani d . 1 1 . . C C8 0.86948(13) 0.08980(16) 0.65915(9) 0.0213(4) Uani d . 1 1 . . C C9 0.78567(13) 0.11498(19) 0.76513(9) 0.0236(4) Uani d . 1 1 . . H H9A 0.7265 0.1524 0.7427 0.028 Uiso calc R 1 1 . . H H9B 0.8007 0.1721 0.8015 0.028 Uiso calc R 1 1 . . C C10 0.75793(15) -0.0231(2) 0.78918(10) 0.0298(4) Uani d . 1 1 . . H H10A 0.6989 -0.0174 0.8171 0.045 Uiso calc R 1 1 . . H H10B 0.8156 -0.0599 0.8123 0.045 Uiso calc R 1 1 . . H H10C 0.7417 -0.0798 0.7534 0.045 Uiso calc R 1 1 . . C C11 0.97664(13) 0.14064(18) 0.75210(9) 0.0246(4) Uani d . 1 1 . . H H11A 1.0310 0.0973 0.7277 0.029 Uiso calc R 1 1 . . H H11B 0.9768 0.1028 0.7949 0.029 Uiso calc R 1 1 . . C C12 0.99913(15) 0.28917(19) 0.75623(10) 0.0296(5) Uani d . 1 1 . . H H12A 1.0650 0.3028 0.7766 0.044 Uiso calc R 1 1 . . H H12B 0.9459 0.3322 0.7808 0.044 Uiso calc R 1 1 . . H H12C 1.0008 0.3265 0.7138 0.044 Uiso calc R 1 1 . . C C13 0.22137(16) 0.1077(3) 0.52797(11) 0.0401(5) Uani d . 1 1 . . H H13A 0.1567 0.0654 0.5177 0.060 Uiso calc R 1 1 . . H H13B 0.2457 0.1569 0.4914 0.060 Uiso calc R 1 1 . . H H13C 0.2116 0.1676 0.5634 0.060 Uiso calc R 1 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0251(3) 0.0307(3) 0.0347(3) -0.00535(18) 0.00843(18) -0.00309(18) O1 0.0258(7) 0.0211(7) 0.0378(8) -0.0015(5) -0.0037(6) 0.0012(5) O2 0.0193(7) 0.0438(9) 0.0351(8) -0.0006(6) -0.0042(5) 0.0002(6) N1 0.0196(7) 0.0170(8) 0.0265(8) -0.0021(5) -0.0025(6) -0.0007(6) N2 0.0188(7) 0.0181(7) 0.0275(8) -0.0002(5) -0.0016(6) 0.0003(6) C1 0.0273(10) 0.0215(10) 0.0238(10) 0.0017(7) 0.0004(7) 0.0011(7) C2 0.0255(9) 0.0315(11) 0.0244(9) 0.0085(8) -0.0015(7) 0.0035(7) C3 0.0207(9) 0.0348(11) 0.0184(9) 0.0003(7) 0.0004(6) -0.0014(7) C4 0.0242(9) 0.0227(9) 0.0239(10) -0.0025(7) 0.0016(7) -0.0026(7) C5 0.0209(9) 0.0240(9) 0.0212(9) 0.0018(7) 0.0021(6) 0.0005(7) C6 0.0210(9) 0.0206(9) 0.0187(8) 0.0009(7) 0.0016(6) -0.0006(6) C7 0.0226(9) 0.0184(9) 0.0197(8) -0.0012(7) 0.0022(6) 0.0008(6) C8 0.0194(9) 0.0149(9) 0.0295(10) 0.0000(6) -0.0012(7) 0.0010(6) C9 0.0220(9) 0.0222(9) 0.0265(10) 0.0007(7) 0.0001(7) -0.0027(7) C10 0.0261(10) 0.0314(11) 0.0318(10) -0.0026(8) 0.0028(8) 0.0030(8) C11 0.0204(9) 0.0211(10) 0.0323(10) 0.0008(7) -0.0066(7) 0.0002(7) C12 0.0252(9) 0.0268(11) 0.0367(11) -0.0050(7) -0.0082(8) 0.0024(8) C13 0.0229(10) 0.0591(15) 0.0384(12) 0.0080(9) -0.0058(8) 0.0033(10) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C8 . 1.6663(18) ? O1 C7 . 1.237(2) ? O2 C3 . 1.367(2) ? O2 C13 . 1.428(3) ? N1 C7 . 1.351(2) ? N1 C8 . 1.431(2) ? N1 H1A . 0.8600 ? N2 C8 . 1.327(2) ? N2 C11 . 1.470(2) ? N2 C9 . 1.479(2) ? C1 C2 . 1.394(3) ? C1 C6 . 1.395(3) ? C1 H1B . 0.9300 ? C2 C3 . 1.387(3) ? C2 H2A . 0.9300 ? C3 C4 . 1.397(3) ? C4 C5 . 1.379(3) ? C4 H4A . 0.9300 ? C5 C6 . 1.396(3) ? C5 H5A . 0.9300 ? C6 C7 . 1.490(2) ? C9 C10 . 1.514(3) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 H10A . 0.9600 ? C10 H10B . 0.9600 ? C10 H10C . 0.9600 ? C11 C12 . 1.517(3) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? C13 H13A . 0.9600 ? C13 H13B . 0.9600 ? C13 H13C . 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 O2 C13 . . 117.56(17) ? C7 N1 C8 . . 120.83(15) ? C7 N1 H1A . . 119.6 ? C8 N1 H1A . . 119.6 ? C8 N2 C11 . . 121.01(15) ? C8 N2 C9 . . 123.58(14) ? C11 N2 C9 . . 115.40(14) ? C2 C1 C6 . . 121.00(17) ? C2 C1 H1B . . 119.5 ? C6 C1 H1B . . 119.5 ? C3 C2 C1 . . 119.34(17) ? C3 C2 H2A . . 120.3 ? C1 C2 H2A . . 120.3 ? O2 C3 C2 . . 124.80(17) ? O2 C3 C4 . . 115.01(17) ? C2 C3 C4 . . 120.19(17) ? C5 C4 C3 . . 119.97(18) ? C5 C4 H4A . . 120.0 ? C3 C4 H4A . . 120.0 ? C4 C5 C6 . . 120.81(17) ? C4 C5 H5A . . 119.6 ? C6 C5 H5A . . 119.6 ? C1 C6 C5 . . 118.69(17) ? C1 C6 C7 . . 117.74(16) ? C5 C6 C7 . . 123.43(16) ? O1 C7 N1 . . 120.50(16) ? O1 C7 C6 . . 121.81(16) ? N1 C7 C6 . . 117.60(15) ? N2 C8 N1 . . 114.73(15) ? N2 C8 S1 . . 126.08(14) ? N1 C8 S1 . . 119.16(13) ? N2 C9 C10 . . 112.64(15) ? N2 C9 H9A . . 109.1 ? C10 C9 H9A . . 109.1 ? N2 C9 H9B . . 109.1 ? C10 C9 H9B . . 109.1 ? H9A C9 H9B . . 107.8 ? C9 C10 H10A . . 109.5 ? C9 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C9 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? N2 C11 C12 . . 111.73(14) ? N2 C11 H11A . . 109.3 ? C12 C11 H11A . . 109.3 ? N2 C11 H11B . . 109.3 ? C12 C11 H11B . . 109.3 ? H11A C11 H11B . . 107.9 ? C11 C12 H12A . . 109.5 ? C11 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C11 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? O2 C13 H13A . . 109.5 ? O2 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? O2 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -0.2(3) ? C13 O2 C3 C2 . . . . -0.6(3) ? C13 O2 C3 C4 . . . . 179.54(17) ? C1 C2 C3 O2 . . . . 179.78(17) ? C1 C2 C3 C4 . . . . -0.3(3) ? O2 C3 C4 C5 . . . . -179.75(16) ? C2 C3 C4 C5 . . . . 0.3(3) ? C3 C4 C5 C6 . . . . 0.2(3) ? C2 C1 C6 C5 . . . . 0.8(3) ? C2 C1 C6 C7 . . . . -175.01(16) ? C4 C5 C6 C1 . . . . -0.8(3) ? C4 C5 C6 C7 . . . . 174.78(16) ? C8 N1 C7 O1 . . . . -4.6(3) ? C8 N1 C7 C6 . . . . 178.96(15) ? C1 C6 C7 O1 . . . . 5.0(3) ? C5 C6 C7 O1 . . . . -170.57(16) ? C1 C6 C7 N1 . . . . -178.57(16) ? C5 C6 C7 N1 . . . . 5.9(2) ? C11 N2 C8 N1 . . . . 176.34(14) ? C9 N2 C8 N1 . . . . -2.8(2) ? C11 N2 C8 S1 . . . . -1.5(2) ? C9 N2 C8 S1 . . . . 179.41(13) ? C7 N1 C8 N2 . . . . 84.6(2) ? C7 N1 C8 S1 . . . . -97.46(17) ? C8 N2 C9 C10 . . . . 84.7(2) ? C11 N2 C9 C10 . . . . -94.45(18) ? C8 N2 C11 C12 . . . . 94.1(2) ? C9 N2 C11 C12 . . . . -86.69(19) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O1 . . 7_645 0.86 2.05 2.847(2) 154 yes _iucr_refine_instructions_details ; TITL A in Pbca CELL 1.54178 12.9024 10.0095 20.8585 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0004 0.0011 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O S UNIT 104 144 16 16 8 L.S. 34 ACTA BOND $H FMAP 2 2 60 PLAN 20 CONF SIZE 0.24 0.1 0.05 TEMP WGHT 0.083100 0.614300 FVAR 0.10025 S1 5 0.967732 0.088651 0.607312 11.00000 0.02512 0.03072 = 0.03466 -0.00309 0.00843 -0.00535 O1 4 0.721742 0.273963 0.630456 11.00000 0.02576 0.02107 = 0.03783 0.00125 -0.00368 -0.00150 O2 4 0.295905 0.008392 0.544915 11.00000 0.01930 0.04378 = 0.03514 0.00022 -0.00417 -0.00061 N1 3 0.767586 0.057754 0.636913 11.00000 0.01955 0.01700 = 0.02648 -0.00070 -0.00253 -0.00210 AFIX 43 H1A 2 0.749469 -0.024570 0.633217 11.00000 -1.20000 AFIX 0 N2 3 0.876085 0.114145 0.721559 11.00000 0.01877 0.01810 = 0.02749 0.00028 -0.00160 -0.00017 C1 1 0.525753 0.214055 0.580558 11.00000 0.02736 0.02146 = 0.02377 0.00109 0.00043 0.00172 AFIX 43 H1B 2 0.547180 0.302758 0.581135 11.00000 -1.20000 AFIX 0 C2 1 0.424483 0.183378 0.562525 11.00000 0.02549 0.03152 = 0.02438 0.00354 -0.00151 0.00851 AFIX 43 H2A 2 0.378538 0.251039 0.551301 11.00000 -1.20000 AFIX 0 C3 1 0.392925 0.050937 0.561489 11.00000 0.02071 0.03479 = 0.01837 -0.00143 0.00042 0.00031 C4 1 0.462280 -0.050503 0.578057 11.00000 0.02420 0.02268 = 0.02393 -0.00261 0.00157 -0.00252 AFIX 43 H4A 2 0.441027 -0.139261 0.577098 11.00000 -1.20000 AFIX 0 C5 1 0.562283 -0.018981 0.595839 11.00000 0.02091 0.02400 = 0.02118 0.00048 0.00207 0.00182 AFIX 43 H5A 2 0.608185 -0.086957 0.606687 11.00000 -1.20000 AFIX 0 C6 1 0.595454 0.113698 0.597754 11.00000 0.02100 0.02062 = 0.01868 -0.00064 0.00158 0.00089 C7 1 0.699444 0.155216 0.621643 11.00000 0.02257 0.01842 = 0.01975 0.00076 0.00216 -0.00121 C8 1 0.869476 0.089806 0.659151 11.00000 0.01943 0.01493 = 0.02951 0.00095 -0.00120 0.00002 C9 1 0.785666 0.114984 0.765131 11.00000 0.02202 0.02222 = 0.02654 -0.00269 0.00011 0.00070 AFIX 23 H9A 2 0.726533 0.152428 0.742730 11.00000 -1.20000 H9B 2 0.800681 0.172145 0.801517 11.00000 -1.20000 AFIX 0 C10 1 0.757933 -0.023148 0.789184 11.00000 0.02614 0.03137 = 0.03181 0.00297 0.00282 -0.00261 AFIX 33 H10A 2 0.698927 -0.017369 0.817083 11.00000 -1.50000 H10B 2 0.815606 -0.059909 0.812301 11.00000 -1.50000 H10C 2 0.741679 -0.079768 0.753422 11.00000 -1.50000 AFIX 0 C11 1 0.976645 0.140640 0.752104 11.00000 0.02042 0.02107 = 0.03226 0.00019 -0.00663 0.00075 AFIX 23 H11A 2 1.031034 0.097265 0.727661 11.00000 -1.20000 H11B 2 0.976763 0.102808 0.794918 11.00000 -1.20000 AFIX 0 C12 1 0.999127 0.289172 0.756226 11.00000 0.02523 0.02680 = 0.03669 0.00241 -0.00822 -0.00496 AFIX 33 H12A 2 1.064999 0.302774 0.776607 11.00000 -1.50000 H12B 2 0.945860 0.332227 0.780838 11.00000 -1.50000 H12C 2 1.000747 0.326498 0.713842 11.00000 -1.50000 AFIX 0 C13 1 0.221369 0.107710 0.527971 11.00000 0.02289 0.05907 = 0.03841 0.00331 -0.00582 0.00795 AFIX 33 H13A 2 0.156702 0.065375 0.517703 11.00000 -1.50000 H13B 2 0.245694 0.156884 0.491434 11.00000 -1.50000 H13C 2 0.211588 0.167659 0.563384 11.00000 -1.50000 HKLF 4 REM A in Pbca REM R1 = 0.0416 for 2214 Fo > 4sig(Fo) and 0.0484 for all 2548 data REM 163 parameters refined using 0 restraints END WGHT 0.0831 0.6143 REM Highest difference peak 0.427, deepest hole -0.324, 1-sigma level 0.063 Q1 1 0.9204 0.0958 0.6353 11.00000 0.05 0.43 Q2 1 0.6402 0.1225 0.6145 11.00000 0.05 0.34 Q3 1 0.4231 0.0032 0.5794 11.00000 0.05 0.30 Q4 1 0.5940 0.0523 0.5849 11.00000 0.05 0.28 Q5 1 0.8327 0.1260 0.7436 11.00000 0.05 0.27 Q6 1 0.5607 0.1547 0.5915 11.00000 0.05 0.27 Q7 1 0.5203 -0.0225 0.5807 11.00000 0.05 0.26 Q8 1 0.9267 0.1332 0.7365 11.00000 0.05 0.26 Q9 1 0.8831 0.0586 0.7012 11.00000 0.05 0.25 Q10 1 1.0188 0.1097 0.6393 11.00000 0.05 0.23 ; data_global _journal_date_recd_electronic 2011-11-17 _journal_date_accepted 2011-11-18 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2011 _journal_volume 67 _journal_issue 12 _journal_page_first o3414 _journal_page_last o3414 _journal_paper_category QO _journal_coeditor_code GK2435 _publ_contact_author_name 'Kassim, Mohammad B.' _publ_contact_author_address ; School of Chemical Sciences and Food Technology Universiti Kebangsaan Malaysia UKM 43600 Bangi Selangor, Malaysia ; _publ_contact_author_email 'mbkassim@ukm.my' _publ_contact_author_fax '+603 89215410' _publ_contact_author_phone '+603 89213980' _publ_section_title ; 1,1-Diethyl-3-(4-methoxybenzoyl)thiourea ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Al-abbasi, Aisha A.' . ; School of Chemical Sciences & Food Technology Faculty of Science & Technology Universiti Kebangsaan Malaysia 43600 Bangi, Selangor Malaysia ; 'Mohamed Tahir, Mohamed Ibrahim' . ; Department of Chemistry Faculty of Science Universiti Putra Malaysia 43400 UPM Serdang, Selangor Malaysia ; 'Kassim, Mohammad B.' . ; School of Chemical Sciences and Food Technology Faculty of Science and Technology Universiti Kebangsaan Malaysia 43600 Selangor Malaysia and Fuel Cell Institute Universiti Kebangsaan Malaysia 43600 Selangor Malaysia ; _publ_section_synopsis .