#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 9 _journal_issue 3 _journal_year 2018 _journal_page_first 151 _journal_page_last 160 #=============================================================================== data_560 _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H6 N2 O' _chemical_formula_sum 'C5 H6 N2 O' _chemical_formula_weight 110.12 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' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 6.93380(10) _cell_length_b 11.21090(10) _cell_length_c 13.73190(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1067.44(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14740 _cell_measurement_theta_min 5.0680 _cell_measurement_theta_max 70.0790 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_F_000 464 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.827 _shelx_estimated_absorpt_T_min 0.852 _shelx_estimated_absorpt_T_max 0.960 _exptl_absorpt_correction_T_min 0.79518 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'hybrid pixel detector' _diffrn_detector_area_resol_mean 10 _diffrn_detector_dtime 0.000 _diffrn_detector_type 'Rigaku, HyPix 6000' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer' _diffrn_measurement_device_type ; Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen loops' _diffrn_radiation_collimation 0.3 _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'Cu K\a' _diffrn_source 'Rotating anode' _diffrn_source_type 'Rigaku 007 HF' _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _diffrn_source_current 30.0 _diffrn_source_target Cu _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_number 18404 _diffrn_reflns_av_unetI/netI 0.0153 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.093 _diffrn_reflns_theta_max 68.199 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 1945 _reflns_number_gt 1936 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.916 _reflns_Friedel_fraction_max 0.996 _reflns_Friedel_fraction_full 0.996 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)' _computing_cell_refinement 'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)' _computing_structure_solution ; Oscail (McArdle et al., 2004), SHELXT (Sheldrick, 2015) ; _computing_structure_refinement ; Oscail (McArdle et al., 2004), ShelXle (H\"ubschle et al., 2011) SHELXL-2017/1 (Sheldrick, 2017) ; _computing_molecular_graphics ' Mercury (Macrae et al, 2006)' _computing_publication_material ; Oscail (McArdle et al., 2004), SHELXL-2017/1 (Sheldrick, 2017) PLATON (Spek, 2009) ; _refine_special_details ; Refined as a 2-component perfect inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.1996P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as a perfect inversion twin. ; _refine_ls_abs_structure_Flack 0.5 _chemical_absolute_configuration ? _refine_ls_number_reflns 1945 _refine_ls_number_parameters 161 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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_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 O123 O 0.5102(2) 0.29101(12) 0.59198(9) 0.0256(3) Uani 1 1 d . . . . . H123 H 0.505(4) 0.261(3) 0.528(2) 0.056(9) Uiso 1 1 d . . . . . N11 N 0.4366(2) 0.31831(13) 0.78058(11) 0.0206(4) Uani 1 1 d . . . . . H11 H 0.395(3) 0.268(2) 0.7349(19) 0.029(6) Uiso 1 1 d . . . . . N122 N 0.6528(2) 0.37982(14) 0.59193(12) 0.0209(3) Uani 1 1 d . . . . . C12 C 0.5786(3) 0.40308(15) 0.76682(13) 0.0186(4) Uani 1 1 d . . . . . C13 C 0.6099(3) 0.45708(16) 0.85664(14) 0.0211(4) Uani 1 1 d . . . . . H13 H 0.699511 0.519042 0.869997 0.025 Uiso 1 1 calc R U . . . C14 C 0.4850(3) 0.40337(16) 0.92386(14) 0.0229(4) Uani 1 1 d . . . . . H14 H 0.475072 0.422449 0.991077 0.028 Uiso 1 1 calc R U . . . C15 C 0.3793(3) 0.31827(17) 0.87544(14) 0.0237(4) Uani 1 1 d . . . . . H15 H 0.283333 0.268283 0.903222 0.028 Uiso 1 1 calc R U . . . C121 C 0.6746(3) 0.42777(16) 0.67625(14) 0.0199(4) Uani 1 1 d . . . . . H121 H 0.768893 0.489139 0.679166 0.024 Uiso 1 1 calc R U . . . O223 O 0.84063(19) 0.40665(11) 0.41656(10) 0.0222(3) Uani 1 1 d . . . . . H223 H 0.775(4) 0.400(2) 0.479(2) 0.051(8) Uiso 1 1 d . . . . . N21 N 0.8573(2) 0.44532(13) 0.22575(11) 0.0193(3) Uani 1 1 d . . . . . H21 H 0.799(4) 0.480(2) 0.278(2) 0.035(7) Uiso 1 1 d . . . . . N222 N 0.9541(2) 0.30325(13) 0.41100(11) 0.0202(3) Uani 1 1 d . . . . . C22 C 0.9660(2) 0.34267(16) 0.23415(13) 0.0179(4) Uani 1 1 d . . . . . C23 C 1.0240(3) 0.31085(17) 0.14105(13) 0.0202(4) Uani 1 1 d . . . . . H23 H 1.101217 0.243899 0.124337 0.024 Uiso 1 1 calc R U . . . C24 C 0.9482(3) 0.39531(17) 0.07586(15) 0.0222(4) Uani 1 1 d . . . . . H24 H 0.964273 0.395764 0.007151 0.027 Uiso 1 1 calc R U . . . C25 C 0.8465(3) 0.47722(18) 0.12993(14) 0.0215(4) Uani 1 1 d . . . . . H25 H 0.779931 0.544620 0.104839 0.026 Uiso 1 1 calc R U . . . C221 C 1.0074(3) 0.28051(16) 0.32360(14) 0.0192(4) Uani 1 1 d . . . . . H221 H 1.086645 0.211898 0.316689 0.023 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 O123 0.0294(7) 0.0289(7) 0.0187(8) -0.0055(6) 0.0008(6) -0.0087(5) N11 0.0212(8) 0.0227(7) 0.0178(8) -0.0012(6) 0.0003(7) -0.0020(6) N122 0.0201(7) 0.0225(7) 0.0201(8) -0.0005(6) 0.0022(7) -0.0002(6) C12 0.0187(9) 0.0199(8) 0.0172(10) 0.0009(7) -0.0016(7) 0.0020(7) C13 0.0232(9) 0.0201(8) 0.0202(9) -0.0024(7) -0.0022(8) 0.0007(7) C14 0.0279(10) 0.0251(10) 0.0157(9) -0.0007(7) 0.0001(8) 0.0053(7) C15 0.0245(9) 0.0256(9) 0.0210(9) 0.0037(7) 0.0052(8) 0.0005(8) C121 0.0195(8) 0.0214(8) 0.0190(9) 0.0011(8) 0.0005(7) -0.0004(7) O223 0.0258(7) 0.0226(6) 0.0181(7) 0.0006(5) 0.0035(6) 0.0038(5) N21 0.0193(7) 0.0222(8) 0.0163(8) 0.0005(6) 0.0009(6) 0.0015(6) N222 0.0204(7) 0.0220(8) 0.0182(8) 0.0022(6) -0.0008(6) 0.0012(6) C22 0.0168(8) 0.0201(8) 0.0168(9) 0.0000(7) 0.0003(7) -0.0013(6) C23 0.0185(8) 0.0215(9) 0.0204(10) -0.0015(7) 0.0000(7) -0.0015(7) C24 0.0227(8) 0.0278(9) 0.0161(9) 0.0007(7) -0.0008(7) -0.0052(7) C25 0.0211(9) 0.0243(9) 0.0191(9) 0.0046(7) -0.0033(7) -0.0009(7) C221 0.0169(8) 0.0214(9) 0.0195(9) 0.0018(7) -0.0002(7) 0.0005(7) _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 O123 N122 1.403(2) . ? O123 H123 0.94(3) . ? N11 C15 1.362(2) . ? N11 C12 1.381(2) . ? N11 H11 0.89(3) . ? N122 C121 1.286(3) . ? C12 C13 1.391(2) . ? C12 C121 1.437(3) . ? C13 C14 1.402(3) . ? C13 H13 0.9500 . ? C14 C15 1.374(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C121 H121 0.9500 . ? O223 N222 1.4030(19) . ? O223 H223 0.97(3) . ? N21 C25 1.366(2) . ? N21 C22 1.381(2) . ? N21 H21 0.92(3) . ? N222 C221 1.281(3) . ? C22 C23 1.387(3) . ? C22 C221 1.441(3) . ? C23 C24 1.405(3) . ? C23 H23 0.9500 . ? C24 C25 1.376(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C221 H221 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 N122 O123 H123 107(2) . . ? C15 N11 C12 109.82(16) . . ? C15 N11 H11 125.6(16) . . ? C12 N11 H11 124.5(16) . . ? C121 N122 O123 112.27(15) . . ? N11 C12 C13 106.80(16) . . ? N11 C12 C121 125.51(16) . . ? C13 C12 C121 127.69(16) . . ? C12 C13 C14 107.50(16) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? C15 C14 C13 108.00(17) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? N11 C15 C14 107.87(17) . . ? N11 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? N122 C121 C12 130.12(16) . . ? N122 C121 H121 114.9 . . ? C12 C121 H121 114.9 . . ? N222 O223 H223 104.5(16) . . ? C25 N21 C22 109.19(16) . . ? C25 N21 H21 128.6(15) . . ? C22 N21 H21 122.1(15) . . ? C221 N222 O223 112.16(15) . . ? N21 C22 C23 107.20(16) . . ? N21 C22 C221 125.67(16) . . ? C23 C22 C221 127.13(16) . . ? C22 C23 C24 107.79(17) . . ? C22 C23 H23 126.1 . . ? C24 C23 H23 126.1 . . ? C25 C24 C23 107.33(18) . . ? C25 C24 H24 126.3 . . ? C23 C24 H24 126.3 . . ? N21 C25 C24 108.49(17) . . ? N21 C25 H25 125.8 . . ? C24 C25 H25 125.8 . . ? N222 C221 C22 130.14(17) . . ? N222 C221 H221 114.9 . . ? C22 C221 H221 114.9 . . ? 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 C15 N11 C12 C13 0.1(2) . . . . ? C15 N11 C12 C121 179.43(17) . . . . ? N11 C12 C13 C14 0.0(2) . . . . ? C121 C12 C13 C14 -179.31(17) . . . . ? C12 C13 C14 C15 -0.1(2) . . . . ? C12 N11 C15 C14 -0.1(2) . . . . ? C13 C14 C15 N11 0.2(2) . . . . ? O123 N122 C121 C12 0.7(3) . . . . ? N11 C12 C121 N122 -0.1(3) . . . . ? C13 C12 C121 N122 179.12(19) . . . . ? C25 N21 C22 C23 0.2(2) . . . . ? C25 N21 C22 C221 -178.98(17) . . . . ? N21 C22 C23 C24 -0.3(2) . . . . ? C221 C22 C23 C24 178.85(17) . . . . ? C22 C23 C24 C25 0.3(2) . . . . ? C22 N21 C25 C24 0.0(2) . . . . ? C23 C24 C25 N21 -0.2(2) . . . . ? O223 N222 C221 C22 -1.1(3) . . . . ? N21 C22 C221 N222 1.1(3) . . . . ? C23 C22 C221 N222 -177.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O123 H123 N222 0.94(3) 1.80(3) 2.7283(19) 171(3) 3_455 yes N11 H11 O123 0.89(3) 2.13(3) 2.657(2) 117.1(19) . yes O223 H223 N122 0.97(3) 1.78(3) 2.754(2) 177(2) . yes N21 H21 O223 0.92(3) 2.09(3) 2.658(2) 119.1(19) . yes C221 H221 O223 0.95 2.60 3.372(2) 138.9 3 yes _refine_diff_density_max 0.128 _refine_diff_density_min -0.150 _refine_diff_density_rms 0.029 _shelx_res_file ; TITL 560_a.res in Pna2(1) 560.res created by SHELXL-2017/1 at 17:21:57 on 26-Sep-2017 REM Old TITL 2017ncs0560a in Pna2(1) REM SHELXT solution in Pna2(1) REM R1 0.065, Rweak 0.005, Alpha 0.001, Orientation as input REM Flack x = 0.209 ( 0.062 ) from Parsons' quotients REM Formula found by SHELXT: C10 N4 O2 CELL 1.54184 6.9338 11.2109 13.7319 90.000 90.000 90.000 ZERR 8.000 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, 1/2+Z SFAC C H N O UNIT 40 48 16 8 TEMP -173 SIZE 0.20 0.15 0.05 L.S. 10 BOND $H CONF ACTA EQIV $1 x-1/2, -y+1/2, z HTAB O123 N222_$1 HTAB N11 O123 HTAB O223 N122 HTAB N21 O223 EQIV $2 x+1/2, -y+1/2, z HTAB C221 O223_$2 LIST 4 FMAP 2 PLAN 20 TWIN WGHT 0.037500 0.199600 FVAR 1.12421 O123 4 0.510180 0.291007 0.591976 11.00000 0.02936 0.02889 = 0.01868 -0.00547 0.00078 -0.00866 H123 2 0.505041 0.260582 0.528404 11.00000 0.05577 N11 3 0.436628 0.318309 0.780583 11.00000 0.02121 0.02266 = 0.01784 -0.00124 0.00034 -0.00203 H11 2 0.395407 0.268425 0.734938 11.00000 0.02862 N122 3 0.652814 0.379817 0.591928 11.00000 0.02009 0.02245 = 0.02010 -0.00046 0.00219 -0.00021 C12 1 0.578617 0.403085 0.766817 11.00000 0.01873 0.01988 = 0.01720 0.00088 -0.00156 0.00203 C13 1 0.609871 0.457078 0.856644 11.00000 0.02316 0.02006 = 0.02023 -0.00241 -0.00216 0.00068 AFIX 43 H13 2 0.699511 0.519042 0.869997 11.00000 -1.20000 AFIX 0 C14 1 0.484967 0.403374 0.923856 11.00000 0.02792 0.02515 = 0.01574 -0.00072 0.00009 0.00526 AFIX 43 H14 2 0.475072 0.422449 0.991077 11.00000 -1.20000 AFIX 0 C15 1 0.379317 0.318270 0.875442 11.00000 0.02448 0.02563 = 0.02097 0.00375 0.00517 0.00054 AFIX 43 H15 2 0.283333 0.268283 0.903222 11.00000 -1.20000 AFIX 0 C121 1 0.674590 0.427770 0.676252 11.00000 0.01947 0.02135 = 0.01903 0.00112 0.00054 -0.00044 AFIX 43 H121 2 0.768893 0.489139 0.679166 11.00000 -1.20000 AFIX 0 O223 4 0.840632 0.406646 0.416564 11.00000 0.02581 0.02262 = 0.01807 0.00060 0.00348 0.00376 H223 2 0.774875 0.400272 0.479020 11.00000 0.05075 N21 3 0.857255 0.445323 0.225746 11.00000 0.01933 0.02222 = 0.01626 0.00047 0.00090 0.00149 H21 2 0.799003 0.480270 0.278393 11.00000 0.03549 N222 3 0.954108 0.303255 0.411001 11.00000 0.02036 0.02201 = 0.01823 0.00216 -0.00082 0.00119 C22 1 0.966033 0.342668 0.234155 11.00000 0.01676 0.02008 = 0.01684 0.00004 0.00027 -0.00128 C23 1 1.024025 0.310849 0.141050 11.00000 0.01854 0.02153 = 0.02043 -0.00152 0.00000 -0.00146 AFIX 43 H23 2 1.101217 0.243899 0.124337 11.00000 -1.20000 AFIX 0 C24 1 0.948225 0.395310 0.075856 11.00000 0.02266 0.02782 = 0.01610 0.00065 -0.00084 -0.00520 AFIX 43 H24 2 0.964273 0.395764 0.007151 11.00000 -1.20000 AFIX 0 C25 1 0.846477 0.477222 0.129928 11.00000 0.02114 0.02426 = 0.01906 0.00464 -0.00330 -0.00090 AFIX 43 H25 2 0.779931 0.544620 0.104839 11.00000 -1.20000 AFIX 0 C221 1 1.007411 0.280509 0.323602 11.00000 0.01689 0.02136 = 0.01948 0.00184 -0.00020 0.00055 AFIX 43 H221 2 1.086645 0.211898 0.316689 11.00000 -1.20000 REM ##### REM ##### REM ##### AFIX 0 HKLF 4 REM 560_a.res in Pna2(1) REM R1 = 0.0238 for 1936 Fo > 4sig(Fo) and 0.0239 for all 1945 data REM 161 parameters refined using 1 restraints END WGHT 0.0382 0.2040 REM Highest difference peak 0.128, deepest hole -0.150, 1-sigma level 0.029 Q1 1 0.6899 0.4134 0.5521 11.00000 0.05 0.13 Q2 1 1.0131 0.3184 0.1950 11.00000 0.05 0.13 Q3 1 1.0031 0.2765 0.4570 11.00000 0.05 0.11 Q4 1 0.5344 0.3605 0.7631 11.00000 0.05 0.10 Q5 1 0.9282 0.3967 0.2375 11.00000 0.05 0.10 Q6 1 0.8292 0.4458 0.3385 11.00000 0.05 0.10 Q7 1 0.9788 0.3106 0.2734 11.00000 0.05 0.10 Q8 1 0.6718 0.6223 0.0636 11.00000 0.05 0.09 Q9 1 0.5661 0.4408 0.8046 11.00000 0.05 0.09 Q10 1 0.6328 0.4092 0.7254 11.00000 0.05 0.09 Q11 1 0.5577 0.4241 0.8973 11.00000 0.05 0.09 Q12 1 1.0084 0.4397 0.4364 11.00000 0.05 0.09 Q13 1 0.6214 0.4198 0.8093 11.00000 0.05 0.09 Q14 1 0.7696 0.5727 0.1320 11.00000 0.05 0.09 Q15 1 1.0231 0.4572 0.4538 11.00000 0.05 0.08 Q16 1 0.6594 0.4008 0.4183 11.00000 0.05 0.08 Q17 1 0.2911 0.2180 0.8811 11.00000 0.05 0.08 Q18 1 0.8091 0.3023 0.0172 11.00000 0.05 0.08 Q19 1 0.3567 0.4594 0.9851 11.00000 0.05 0.08 Q20 1 0.6476 0.3567 0.9069 11.00000 0.05 0.08 ; _shelx_res_checksum 46483 _shelx_hkl_file ; 0 0 -16 207.89 8.72 0 0 -16 211.52 8.81 0 0 -16 242.86 9.01 0 0 -16 245.01 8.77 0 0 -15 0.25 1.04 0 0 -15 1.65 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4 -4 744.91 23.85 0 4 -4 743.09 23.46 0 -4 -4 743.69 23.61 0 -4 -3 0.49 0.32 0 4 -3 0.73 0.44 0 4 -3 0.23 0.27 0 -4 -3 0.39 0.43 0 -4 -2 352.89 10.77 0 4 -2 327.12 9.96 0 -4 -2 346.16 10.80 0 -4 -2 326.85 10.05 0 -4 -1 0.07 0.38 0 4 0 886.82 26.51 0 -4 0 871.77 26.48 0 -4 1 -0.07 0.38 0 -4 2 326.46 9.92 0 -4 2 346.21 10.71 0 4 2 339.31 10.13 0 4 3 0.32 0.33 0 -4 3 -0.08 0.38 0 4 4 772.80 23.44 0 -4 4 777.48 23.22 0 -4 4 776.86 23.69 0 4 4 733.90 23.91 0 4 4 792.41 24.12 0 4 5 0.10 0.42 0 -4 5 0.49 0.41 0 -4 5 1.64 0.52 0 4 5 0.07 0.62 0 4 5 0.08 0.67 0 4 6 2702.68 80.04 0 4 6 2651.82 78.94 0 -4 6 2669.33 79.07 0 4 6 2681.05 79.42 0 -4 6 2636.91 78.71 0 4 7 0.07 0.48 0 4 7 -0.50 0.72 0 4 7 1.67 1.13 0 -4 7 -0.06 0.45 0 4 8 266.24 10.69 0 4 8 261.05 9.94 0 4 9 0.98 0.85 0 4 9 -0.28 1.08 0 -4 10 199.60 9.34 0 4 10 184.13 7.89 0 4 10 200.88 9.15 0 4 11 0.16 1.32 0 4 11 0.40 0.74 0 -4 11 0.67 1.21 0 -4 12 453.95 17.20 0 4 12 456.97 17.17 0 -4 13 -0.41 1.02 0 4 13 0.44 1.20 0 -4 14 60.30 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0 -5 -3 91.06 3.12 0 5 -3 89.77 4.26 0 5 -3 93.63 3.91 0 -5 -3 87.64 4.79 0 -5 -3 87.11 4.15 0 5 -3 80.89 4.68 0 5 -3 95.08 4.90 0 -5 -3 90.97 4.35 0 5 -3 89.88 4.28 0 -5 -3 96.92 4.02 0 -5 -3 93.14 3.90 0 5 -3 82.45 2.93 0 5 -2 -0.20 0.67 0 -5 -2 0.07 0.62 0 -5 -2 0.05 0.46 0 5 -2 0.07 0.57 0 -5 -2 0.05 0.44 0 -5 -2 0.40 0.69 0 -5 -2 -0.29 0.91 0 5 -2 0.13 0.56 0 5 -2 -0.19 1.02 0 5 -1 69.88 3.36 0 5 -1 67.09 3.34 0 5 -1 66.18 4.12 0 -5 -1 69.64 3.11 0 5 -1 68.38 3.48 0 5 0 0.11 1.03 0 5 0 -0.15 0.78 0 5 0 1.17 0.74 0 5 0 -0.06 0.51 0 5 0 -0.12 0.52 0 -5 0 0.37 0.43 0 5 1 70.33 3.54 0 5 1 65.69 3.64 0 5 1 68.82 3.26 0 -5 1 72.92 3.14 0 5 1 69.63 3.29 0 5 1 69.62 4.42 0 5 2 -0.23 0.96 0 5 2 -0.06 0.57 0 5 2 0.08 0.14 0 -5 2 -0.32 0.72 0 5 2 -0.17 0.59 0 -5 2 0.14 0.41 0 5 2 -0.22 0.74 0 5 3 95.71 4.10 0 5 3 88.29 3.18 0 -5 3 88.95 4.62 0 5 3 91.55 5.23 0 -5 3 95.68 3.85 0 -5 3 85.67 2.89 0 5 3 89.68 4.39 0 5 4 0.14 0.33 0 -5 4 0.10 0.99 0 -5 4 0.06 0.36 0 5 4 -0.07 0.60 0 -5 4 0.14 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1.06 0 7 -6 0.12 0.85 0 7 -6 1.68 1.14 0 7 -6 0.40 0.93 0 -7 -6 -0.13 0.97 0 -7 -6 -0.70 1.28 0 7 -5 117.26 5.92 0 -7 -5 126.07 6.79 0 7 -5 115.18 5.89 0 7 -5 121.15 6.22 0 7 -5 109.14 5.80 0 -7 -5 118.77 5.96 0 7 -5 107.18 5.72 0 7 -5 105.85 6.42 0 -7 -5 112.28 6.52 0 7 -4 0.68 0.93 0 -7 -4 0.91 1.04 0 -7 -4 0.83 0.89 0 7 -4 0.33 1.12 0 7 -4 1.05 1.04 0 7 -4 -0.13 1.08 0 7 -4 1.66 0.94 0 -7 -4 2.23 1.43 0 -7 -4 -0.15 1.05 0 7 -3 1459.97 47.19 0 7 -3 1416.27 44.40 0 -7 -3 1515.79 46.18 0 -7 -3 1507.43 45.71 0 7 -3 1439.01 46.24 0 7 -3 1498.59 45.75 0 7 -3 1449.38 45.50 0 7 -3 1495.50 45.70 0 7 -3 1423.45 46.24 0 7 -3 1483.49 45.78 0 -7 -3 1588.38 47.22 0 7 -2 -0.12 0.95 0 7 -2 -0.09 0.67 0 7 -2 1.15 1.38 0 7 -2 -0.20 0.81 0 7 -2 -0.10 0.87 0 -7 -2 0.10 0.83 0 7 -2 0.79 0.68 0 -7 -2 0.12 0.92 0 7 -2 1.00 0.85 0 7 -2 3.42 1.23 0 -7 -1 418.84 15.38 0 7 -1 415.22 13.86 0 7 -1 392.74 15.44 0 7 -1 422.31 14.02 0 7 -1 413.83 14.63 0 7 -1 423.69 14.73 0 7 -1 413.03 15.22 0 7 -1 415.34 14.41 0 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13.08 0 -11 5 301.06 12.60 0 11 5 335.12 13.13 0 11 5 338.50 12.45 0 11 6 1.09 0.99 0 -11 6 0.42 0.82 0 -11 6 -0.47 1.14 0 11 6 0.13 1.09 0 -11 6 -0.40 1.03 0 11 7 468.33 16.54 0 -11 7 459.81 16.84 0 -11 7 460.59 16.58 0 11 7 458.59 16.00 0 -11 8 0.56 0.90 0 11 8 -0.62 0.97 0 -11 8 0.11 0.86 0 -11 9 145.72 6.40 0 11 9 168.07 6.52 0 11 9 163.70 6.67 0 -11 9 162.76 6.88 0 -12 -7 0.27 0.72 0 12 -7 -0.21 0.58 0 12 -7 -0.07 0.53 0 -12 -7 0.21 0.62 0 12 -6 2.77 0.94 0 -12 -6 2.15 0.87 0 12 -6 3.15 0.95 0 -12 -6 3.19 1.12 0 -12 -5 -0.36 1.03 0 -12 -5 -0.85 0.87 0 12 -5 0.54 0.69 0 12 -4 427.47 14.87 0 -12 -4 425.38 14.77 0 12 -4 443.23 14.92 0 -12 -3 0.11 0.92 0 12 -3 1.62 0.98 0 12 -3 0.88 0.90 0 12 -3 0.67 0.88 0 12 -2 82.12 4.61 0 12 -2 81.85 4.57 0 -12 -2 81.10 4.59 0 12 -2 75.81 4.47 0 -12 -2 74.87 5.03 0 12 -1 0.34 0.92 0 12 -1 0.11 0.86 0 12 -1 0.12 0.99 0 -12 -1 0.11 0.93 0 -12 -1 0.46 1.22 0 -12 0 28.60 2.64 0 -12 0 29.55 2.99 0 12 0 26.55 2.44 0 12 0 29.01 2.54 0 -12 0 27.05 2.94 0 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11.89 1.33 -7 6 3 15.14 1.55 -7 -6 3 13.42 1.58 -7 6 3 14.28 1.52 -7 -6 3 11.11 1.28 7 6 3 11.31 1.52 -7 6 3 10.31 1.30 7 6 4 71.26 3.61 -7 6 4 64.60 3.35 -7 6 5 49.13 2.63 -7 6 5 49.27 2.63 7 6 5 44.11 2.54 7 7 -2 91.18 4.06 -7 -7 -2 94.81 4.61 7 7 -1 88.66 4.17 7 7 -1 110.88 4.39 -7 7 0 20.25 1.53 -7 7 0 17.11 1.44 7 7 0 17.44 1.60 7 7 0 18.22 1.52 -7 -7 0 18.89 1.88 -7 7 1 121.39 4.88 -7 7 1 122.69 4.90 7 7 1 109.76 4.94 -7 -7 1 120.59 5.40 -7 7 2 99.09 4.21 -7 7 2 99.20 4.21 8 0 -4 141.79 5.55 -8 0 -4 139.91 5.76 -8 0 -4 126.35 5.40 8 0 -4 141.53 5.55 8 0 -3 149.90 5.78 -8 0 -3 138.85 6.04 -8 0 -3 139.30 5.88 8 0 -3 146.47 5.75 -8 0 -2 23.00 2.07 -8 0 -2 22.09 1.98 -8 0 -1 198.48 7.93 -8 0 -1 215.79 7.72 -8 0 0 12.19 1.51 -8 0 0 15.23 1.60 -8 0 0 10.49 1.46 -8 0 1 194.89 8.05 -8 0 1 213.89 8.02 -8 0 2 24.55 2.15 -8 0 3 156.23 6.47 -8 0 3 154.59 6.34 -8 0 3 155.14 6.45 -8 0 4 143.63 5.96 -8 0 4 149.45 5.93 -8 0 4 139.90 5.97 8 -1 -4 127.26 5.06 8 1 -4 116.00 4.84 -8 -1 -4 117.78 5.19 8 -1 -4 126.52 5.04 8 1 -4 121.36 4.87 -8 -1 -3 288.30 10.67 8 -1 -3 344.21 10.80 8 1 -3 313.35 10.48 -8 1 -3 307.84 10.79 -8 -1 -3 303.15 10.92 -8 1 -3 274.21 10.43 8 -1 -3 331.96 10.73 8 1 -3 305.87 10.44 8 -1 -2 110.95 4.82 -8 -1 -2 123.39 5.52 -8 1 -2 123.67 5.30 -8 1 -2 109.08 4.75 -8 1 -2 120.99 5.17 -8 -1 -2 119.15 5.34 8 -1 -2 112.59 4.83 -8 1 -1 9.53 1.38 -8 1 -1 12.91 1.39 -8 1 -1 10.85 1.41 -8 -1 -1 13.16 1.49 -8 1 0 13.34 1.62 -8 1 0 17.98 1.69 -8 -1 0 18.29 1.75 -8 1 0 14.56 1.66 -8 1 1 11.94 1.51 -8 1 1 11.02 1.46 -8 -1 1 12.38 1.56 -8 1 1 13.30 1.52 -8 1 2 119.59 5.36 -8 1 2 133.75 5.51 -8 -1 2 133.40 5.53 -8 1 3 319.99 11.39 -8 -1 3 343.19 11.54 -8 1 3 313.49 11.48 -8 -1 3 337.68 11.66 -8 1 4 115.32 5.08 -8 1 4 129.81 5.30 -8 -1 4 124.39 5.20 -8 -1 4 132.71 5.42 8 -2 -4 64.53 3.19 -8 -2 -4 67.18 3.44 -8 -2 -4 60.03 3.20 8 -2 -4 63.42 3.17 -8 -2 -3 64.99 3.45 -8 -2 -3 69.07 3.64 -8 -2 -2 26.46 2.02 -8 -2 -2 27.98 2.26 -8 -2 -1 61.93 3.49 -8 2 -1 46.15 2.84 -8 2 -1 64.09 3.02 -8 -2 -1 74.10 3.50 -8 2 -1 49.35 2.91 -8 -2 -1 62.66 3.46 -8 -2 0 11.96 1.49 -8 2 0 6.94 1.08 -8 2 0 8.94 1.23 -8 -2 0 10.84 1.42 -8 2 0 9.99 1.24 -8 -2 1 59.70 3.46 -8 2 1 63.62 3.24 -8 -2 1 65.14 3.39 -8 2 1 54.14 3.11 -8 -2 1 62.04 3.44 -8 -2 2 32.84 2.42 -8 2 2 30.53 2.17 -8 -2 2 32.51 2.27 -8 2 2 29.60 2.17 -8 -2 2 28.77 2.23 8 2 3 71.07 3.38 -8 -2 3 72.11 3.72 -8 2 3 65.91 3.44 -8 -2 3 70.80 3.51 -8 2 3 66.09 3.46 -8 -2 3 68.18 3.55 -8 -2 4 65.79 3.37 -8 -2 4 64.78 3.14 -8 -2 4 56.63 3.09 -8 -3 -3 98.57 4.49 -8 -3 -3 100.08 4.47 -8 -3 -2 35.39 2.46 -8 -3 -2 40.34 2.54 -8 -3 -1 17.22 1.69 -8 -3 -1 16.19 1.67 -8 -3 0 237.73 8.96 -8 -3 0 244.82 8.78 -8 -3 0 232.39 8.81 -8 -3 1 13.71 1.53 -8 3 1 14.27 1.35 -8 -3 1 15.88 1.59 -8 -3 1 14.55 1.58 8 3 2 41.89 2.51 -8 -3 2 40.73 2.61 -8 3 2 35.92 2.29 -8 -3 2 40.80 2.46 -8 -3 2 35.37 2.37 8 3 3 99.24 4.12 -8 -3 3 98.71 4.36 -8 3 3 87.02 3.99 -8 -3 3 90.53 4.04 -8 -3 3 86.74 4.04 0 0 0 0.00 0.00 TITL 2017ncs0560a in Pna2(1) REM Pna2(1) (#33 in standard setting) CELL 1.54184 6.933760 11.210885 13.731878 90.0000 90.0000 90.0000 ZERR 8.00 0.000060 0.000092 0.000127 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y+1/2, z SYMM -x+1/2, y+1/2, z+1/2 SFAC C H N O UNIT 48.00 40.00 16.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 39294