data_General _audit_creation_date 2016-08-01 _audit_creation_method 'by CrystalStructure 4.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Takehiko Mori' _publ_contact_author_email mori.t.ae@m.titech.ac.jp _publ_contact_author_fax +91-3-5734-2876 _publ_contact_author_phone +91-3-5734-2427 _publ_contact_author_address 'O-okayama, Meguro-ku, Tokyo 152-8552, Japan' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ACS Applied Materials & Interfaces' _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Carrier Charge Polarity in Mixed-Stack Charge-Transfer Crystals Containing Dithienobenzodithiophene (DTBDT) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Kodai Iijima' ; Department of Materials Science and Engineering, Tokyo Institute of Technology, ; ; O-okayama, Meguro-ku, Tokyo 152-8552, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2017). CrystalStructure. Version 4.2. Rigaku Corporation, Tokyo, Japan. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. Siliqi, D. and Spagna R. (2007). J. Appl. Cryst. 40, 609-613. SIR2008 Sheldrick, G.M. (2008) SHELXL Version 2018/1, Acta Cryst. A64, 112-122. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_Cytidine_(Rigaku_Master_for_Mo) #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H14 N4 S4' _chemical_formula_moiety 'C14 H6 S4, C10 H8 N4' _chemical_formula_weight 486.64 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 7.730(3) _cell_length_b 7.8084(13) _cell_length_c 9.4033(14) _cell_angle_alpha 108.145(12) _cell_angle_beta 96.07(2) _cell_angle_gamma 94.06(3) _cell_volume 533.1(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.58 _cell_measurement_theta_max 16.73 _cell_measurement_temperature 298 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 250.00 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.995 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 298 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2632 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_theta_max 25.993 _diffrn_reflns_theta_min 2.666 _diffrn_reflns_theta_full 25.240 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.439 _reflns_number_total 2101 _reflns_number_gt 1009 _reflns_threshold_expression F^2^>2.0\s(F^2^) _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1944 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2580 _refine_ls_wR_factor_gt 0.2003 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2101 _refine_ls_number_parameters 146 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1448P)^2^] 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_diff_density_max 1.21 _refine_diff_density_min -0.52 _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' 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.1246 0.1234 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.7015(3) 0.0092(3) 0.2589(2) 0.0533(7) Uani 1 1 d . . . . . S2 S 0.5720(2) 0.4826(3) 0.17600(19) 0.0456(6) Uani 1 1 d . . . . . N1 N 0.1392(7) 0.2335(7) 0.2985(6) 0.0365(13) Uani 1 1 d . . . . . N2 N 0.2287(9) -0.0428(9) 0.3467(8) 0.0576(18) Uani 1 1 d . . . . . C1 C 0.7449(11) -0.0044(12) 0.0809(10) 0.062(2) Uani 1 1 d . . . . . H1 H 0.790096 -0.103455 0.018309 0.074 Uiso 1 1 calc R U . . . C2 C 0.7082(10) 0.1401(14) 0.0397(9) 0.063(2) Uani 1 1 d . . . . . H2 H 0.723573 0.152116 -0.053606 0.075 Uiso 1 1 calc R U . . . C3 C 0.6428(9) 0.2725(10) 0.1569(7) 0.0448(18) Uani 1 1 d . . . . . C4 C 0.6323(8) 0.2201(9) 0.2840(7) 0.0369(16) Uani 1 1 d . . . . . C5 C 0.5674(8) 0.3526(8) 0.4034(7) 0.0292(14) Uani 1 1 d . . . . . C6 C 0.5278(8) 0.5059(9) 0.3605(7) 0.0325(15) Uani 1 1 d . . . . . C7 C 0.4623(8) 0.6532(9) 0.4532(7) 0.0339(15) Uani 1 1 d . . . . . H7 H 0.438799 0.752376 0.422378 0.041 Uiso 1 1 calc R U . . . C8 C 0.0710(8) 0.3594(8) 0.3984(7) 0.0315(14) Uani 1 1 d . . . . . C9 C 0.0260(8) 0.5175(8) 0.3547(7) 0.0308(14) Uani 1 1 d . . . . . C10 C 0.0411(8) 0.3516(8) 0.5449(7) 0.0310(14) Uani 1 1 d . . . . . H11 H 0.069804 0.250521 0.570767 0.037 Uiso 1 1 calc R U . . . C11 C 0.1846(9) 0.0871(9) 0.3321(7) 0.0391(16) Uani 1 1 d . . . . . C12 C 0.0554(9) 0.5221(9) 0.1993(7) 0.0388(16) Uani 1 1 d . . . . . H12A H 0.031240 0.637480 0.190252 0.047 Uiso 1 1 calc R U . . . H12B H -0.021213 0.427477 0.123967 0.047 Uiso 1 1 calc R U . . . H12C H 0.174773 0.504322 0.185057 0.047 Uiso 1 1 calc R U . . . 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 S1 0.0540(13) 0.0368(11) 0.0587(13) -0.0009(9) 0.0114(10) 0.0065(9) S2 0.0535(12) 0.0605(13) 0.0246(9) 0.0157(8) 0.0065(8) 0.0064(9) N1 0.042(3) 0.031(3) 0.031(3) 0.003(2) 0.003(2) 0.000(2) N2 0.074(5) 0.043(4) 0.056(4) 0.013(3) 0.014(3) 0.009(3) C1 0.061(5) 0.048(5) 0.062(6) -0.006(4) 0.020(4) 0.007(4) C2 0.053(5) 0.084(7) 0.032(4) -0.008(4) 0.013(4) -0.003(5) C3 0.044(4) 0.052(4) 0.029(4) 0.000(3) 0.008(3) -0.002(3) C4 0.038(4) 0.030(3) 0.036(4) 0.001(3) 0.009(3) -0.001(3) C5 0.033(3) 0.026(3) 0.024(3) 0.003(3) 0.002(3) -0.002(3) C6 0.039(4) 0.037(4) 0.021(3) 0.010(3) 0.000(3) 0.000(3) C7 0.040(4) 0.028(3) 0.034(3) 0.011(3) 0.003(3) 0.005(3) C8 0.038(4) 0.027(3) 0.025(3) 0.004(3) 0.003(3) -0.001(3) C9 0.033(4) 0.031(3) 0.027(3) 0.011(3) 0.000(3) -0.002(3) C10 0.038(4) 0.021(3) 0.036(3) 0.013(3) 0.003(3) 0.003(3) C11 0.049(4) 0.031(4) 0.035(4) 0.005(3) 0.009(3) 0.010(3) C12 0.059(4) 0.036(4) 0.029(3) 0.020(3) 0.009(3) 0.006(3) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction WinAFC _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL Version 2018/1 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.2 (Rigaku, 2017)' _computing_molecular_graphics 'CrystalStructure 4.2' #============================================================================== # MOLECULAR GEOMETRY _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 S1 C1 1.714(9) . ? S1 C4 1.721(7) . ? S2 C3 1.728(8) . ? S2 C6 1.760(6) . ? N1 C8 1.315(8) . ? N1 C11 1.337(9) . ? N2 C11 1.137(9) . ? C1 C2 1.341(12) . ? C1 H1 0.9300 . ? C2 C3 1.422(10) . ? C2 H2 0.9300 . ? C3 C4 1.387(10) . ? C4 C5 1.433(8) . ? C5 C7 1.405(9) 2_666 ? C5 C6 1.420(9) . ? C6 C7 1.375(9) . ? C7 H7 0.9300 . ? C8 C10 1.439(9) . ? C8 C9 1.470(9) . ? C9 C10 1.335(9) 2_566 ? C9 C12 1.513(8) . ? C10 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 C1 S1 C4 90.6(4) . . ? C3 S2 C6 91.0(3) . . ? C8 N1 C11 119.2(6) . . ? C2 C1 S1 114.2(6) . . ? C2 C1 H1 122.9 . . ? S1 C1 H1 122.9 . . ? C1 C2 C3 111.4(8) . . ? C1 C2 H2 124.3 . . ? C3 C2 H2 124.3 . . ? C4 C3 C2 112.5(8) . . ? C4 C3 S2 113.0(5) . . ? C2 C3 S2 134.5(7) . . ? C3 C4 C5 113.2(6) . . ? C3 C4 S1 111.3(5) . . ? C5 C4 S1 135.5(5) . . ? C7 C5 C6 119.6(6) 2_666 . ? C7 C5 C4 129.4(6) 2_666 . ? C6 C5 C4 111.0(5) . . ? C7 C6 C5 123.4(6) . . ? C7 C6 S2 124.8(5) . . ? C5 C6 S2 111.8(5) . . ? C6 C7 C5 117.1(6) . 2_666 ? C6 C7 H7 121.5 . . ? C5 C7 H7 121.5 2_666 . ? N1 C8 C10 124.3(6) . . ? N1 C8 C9 116.3(6) . . ? C10 C8 C9 119.4(5) . . ? C10 C9 C8 117.4(6) 2_566 . ? C10 C9 C12 123.8(6) 2_566 . ? C8 C9 C12 118.7(5) . . ? C9 C10 C8 123.2(6) 2_566 . ? C9 C10 H11 118.4 2_566 . ? C8 C10 H11 118.4 . . ? N2 C11 N1 173.1(7) . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 S1 C1 C2 -0.7(7) . . . . ? S1 C1 C2 C3 0.7(10) . . . . ? C1 C2 C3 C4 -0.2(10) . . . . ? C1 C2 C3 S2 -179.6(6) . . . . ? C6 S2 C3 C4 0.5(5) . . . . ? C6 S2 C3 C2 179.9(8) . . . . ? C2 C3 C4 C5 179.7(6) . . . . ? S2 C3 C4 C5 -0.7(7) . . . . ? C2 C3 C4 S1 -0.3(8) . . . . ? S2 C3 C4 S1 179.2(4) . . . . ? C1 S1 C4 C3 0.6(5) . . . . ? C1 S1 C4 C5 -179.5(7) . . . . ? C3 C4 C5 C7 179.4(6) . . . 2_666 ? S1 C4 C5 C7 -0.6(12) . . . 2_666 ? C3 C4 C5 C6 0.6(8) . . . . ? S1 C4 C5 C6 -179.4(5) . . . . ? C7 C5 C6 C7 0.7(11) 2_666 . . . ? C4 C5 C6 C7 179.6(6) . . . . ? C7 C5 C6 S2 -179.1(5) 2_666 . . . ? C4 C5 C6 S2 -0.2(7) . . . . ? C3 S2 C6 C7 180.0(6) . . . . ? C3 S2 C6 C5 -0.2(5) . . . . ? C5 C6 C7 C5 -0.7(11) . . . 2_666 ? S2 C6 C7 C5 179.1(5) . . . 2_666 ? C11 N1 C8 C10 0.1(10) . . . . ? C11 N1 C8 C9 179.3(6) . . . . ? N1 C8 C9 C10 -179.0(6) . . . 2_566 ? C10 C8 C9 C10 0.2(10) . . . 2_566 ? N1 C8 C9 C12 1.8(9) . . . . ? C10 C8 C9 C12 -179.0(5) . . . . ? N1 C8 C10 C9 179.0(6) . . . 2_566 ? C9 C8 C10 C9 -0.2(11) . . . 2_566 ? #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; TITL Cytidine (Rigaku Master for Mo) shelxl.res created by SHELXL-2018/1 at 16:06:38 on 05-Mar-2018 CELL 0.71069 7.72980 7.80840 9.40330 108.14500 96.07020 94.06000 ZERR 1 0.00330 0.00130 0.00140 0.01170 0.02170 0.02540 LATT 1 SFAC C H N S UNIT 24 14 4 4 SHEL 8.146492 0.810603 L.S. 30 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 25.0 ACTA SIZE 0.420 0.040 0.010 WGHT 0.144800 FVAR 0.83194 S1 4 0.701501 0.009238 0.258924 11.00000 0.05402 0.03684 = 0.05873 -0.00091 0.01141 0.00654 S2 4 0.571964 0.482603 0.176004 11.00000 0.05348 0.06049 = 0.02464 0.01568 0.00648 0.00644 N1 3 0.139187 0.233451 0.298467 11.00000 0.04190 0.03136 = 0.03077 0.00343 0.00308 0.00037 N2 3 0.228720 -0.042846 0.346729 11.00000 0.07366 0.04276 = 0.05582 0.01256 0.01445 0.00949 C1 1 0.744937 -0.004382 0.080912 11.00000 0.06117 0.04770 = 0.06219 -0.00613 0.01991 0.00669 AFIX 43 H1 2 0.790096 -0.103455 0.018309 11.00000 -1.20000 AFIX 0 C2 1 0.708202 0.140083 0.039720 11.00000 0.05335 0.08384 = 0.03230 -0.00800 0.01315 -0.00296 AFIX 43 H2 2 0.723573 0.152116 -0.053606 11.00000 -1.20000 AFIX 0 C3 1 0.642763 0.272542 0.156850 11.00000 0.04389 0.05166 = 0.02936 0.00014 0.00755 -0.00173 C4 1 0.632347 0.220110 0.283997 11.00000 0.03844 0.03008 = 0.03569 0.00110 0.00949 -0.00115 C5 1 0.567370 0.352579 0.403449 11.00000 0.03310 0.02614 = 0.02409 0.00345 0.00227 -0.00160 C6 1 0.527786 0.505865 0.360467 11.00000 0.03863 0.03664 = 0.02106 0.00972 0.00014 0.00015 C7 1 0.462347 0.653237 0.453197 11.00000 0.04000 0.02770 = 0.03416 0.01057 0.00335 0.00530 AFIX 43 H7 2 0.438799 0.752376 0.422378 11.00000 -1.20000 AFIX 0 C8 1 0.071010 0.359358 0.398418 11.00000 0.03807 0.02746 = 0.02496 0.00426 0.00255 -0.00060 C9 1 0.025973 0.517495 0.354664 11.00000 0.03348 0.03131 = 0.02679 0.01070 0.00027 -0.00213 C10 1 0.041068 0.351604 0.544852 11.00000 0.03804 0.02133 = 0.03579 0.01272 0.00333 0.00290 AFIX 43 H11 2 0.069804 0.250521 0.570767 11.00000 -1.20000 AFIX 0 C11 1 0.184560 0.087128 0.332064 11.00000 0.04929 0.03059 = 0.03510 0.00493 0.00927 0.01018 C12 1 0.055381 0.522116 0.199285 11.00000 0.05912 0.03616 = 0.02865 0.02021 0.00909 0.00574 AFIX 137 H12A 2 0.031240 0.637480 0.190252 11.00000 -1.20000 H12B 2 -0.021213 0.427477 0.123967 11.00000 -1.20000 H12C 2 0.174773 0.504322 0.185057 11.00000 -1.20000 AFIX 0 HKLF 4 REM Cytidine (Rigaku Master for Mo) REM R1 = 0.0832 for 1009 Fo > 4sig(Fo) and 0.1944 for all 2101 data REM 146 parameters refined using 0 restraints END WGHT 0.1448 0.0000 REM Instructions for potential hydrogen bonds EQIV $3 -x+1, -y, -z HTAB C2 N2_$3 EQIV $4 x, y+1, z HTAB C7 N2_$4 REM Highest difference peak 1.212, deepest hole -0.518, 1-sigma level 0.155 Q1 1 0.4292 0.4980 0.1816 11.00000 0.05 1.21 Q2 1 -0.1333 0.4901 0.1820 11.00000 0.05 0.99 Q3 1 0.7220 0.4900 0.1826 11.00000 0.05 0.94 Q4 1 0.8522 0.0109 0.2628 11.00000 0.05 0.89 Q5 1 0.3076 0.5010 0.1795 11.00000 0.05 0.87 Q6 1 0.5615 0.0102 0.2608 11.00000 0.05 0.82 Q7 1 0.4482 0.0161 0.2598 11.00000 0.05 0.66 Q8 1 0.1773 0.5175 0.3590 11.00000 0.05 0.58 Q9 1 0.7987 0.2429 0.2912 11.00000 0.05 0.51 Q10 1 0.3511 0.2308 0.3034 11.00000 0.05 0.50 Q11 1 0.4128 0.3556 0.3971 11.00000 0.05 0.50 Q12 1 0.8437 0.2386 0.2969 11.00000 0.05 0.49 Q13 1 0.8211 0.3478 0.3997 11.00000 0.05 0.48 Q14 1 0.6874 0.5198 0.3613 11.00000 0.05 0.45 Q15 1 0.2599 0.0049 0.2445 11.00000 0.05 0.45 Q16 1 0.1581 0.3439 0.5707 11.00000 0.05 0.44 Q17 1 -0.0114 -0.0077 0.3598 11.00000 0.05 0.43 Q18 1 0.3255 0.6441 0.4410 11.00000 0.05 0.43 Q19 1 0.7084 0.6392 0.4536 11.00000 0.05 0.42 Q20 1 0.1688 0.4811 0.6454 11.00000 0.05 0.41 Q21 1 0.2169 0.3507 0.4151 11.00000 0.05 0.41 Q22 1 0.6205 0.6599 0.4452 11.00000 0.05 0.40 Q23 1 -0.1183 0.3350 0.5360 11.00000 0.05 0.40 Q24 1 0.0054 0.2377 0.2932 11.00000 0.05 0.40 Q25 1 -0.0930 0.5196 0.3748 11.00000 0.05 0.37 ; _shelx_res_checksum 54584 _shelx_hkl_file ; 0 0 2 2463.17 22.48 0 0 -2 2421.81 22.36 0 0 3 90.84 6.97 0 0 -3 72.69 7.24 0 0 4 74.70 6.96 0 0 -4 61.90 6.03 0 0 5 133.73 12.54 0 0 -5 129.99 12.89 0 0 6 62.03 7.16 0 0 -6 89.40 7.24 0 0 7 -8.29 12.56 0 0 -7 15.21 12.40 0 0 8 75.12 8.53 0 0 -8 88.38 8.82 0 0 9 123.40 10.38 0 0 -9 116.85 10.64 0 0 10 3.09 16.18 0 0 -10 30.43 8.77 0 0 11 78.50 11.25 0 0 -11 82.17 11.28 0 0 12 -30.63 18.39 0 0 -12 9.57 17.03 0 1 -12 20.50 10.03 0 -1 12 20.93 9.50 0 1 -11 50.14 10.18 0 -1 11 -4.85 17.98 0 1 -10 27.26 8.11 0 -1 10 15.42 15.86 0 1 -9 9.57 9.32 0 -1 9 4.27 13.45 0 1 -8 624.90 24.97 0 -1 8 692.24 26.37 0 1 -7 -26.98 12.25 0 -1 7 -5.05 10.92 0 1 -6 449.30 18.77 0 -1 6 442.85 17.85 0 1 -5 2012.55 31.46 0 -1 5 2039.40 31.64 0 1 -4 2286.53 29.10 0 -1 4 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