#============================================================================== 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_557z _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 H4 N2 O4' _chemical_formula_sum 'C5 H4 N2 O4' _chemical_formula_weight 156.10 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' '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.2711(2) _cell_length_b 5.5198(2) _cell_length_c 21.2019(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 616.88(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5820 _cell_measurement_theta_min 1.9000 _cell_measurement_theta_max 33.7430 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_F_000 320 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.149 _shelx_estimated_absorpt_T_min 0.988 _shelx_estimated_absorpt_T_max 0.996 _exptl_absorpt_correction_T_min 0.83531 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _diffrn_radiation_probe x-ray _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RCD3): Kappa single' _diffrn_detector 'CCD plate' _diffrn_reflns_number 8390 _diffrn_reflns_av_unetI/netI 0.0119 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.921 _diffrn_reflns_theta_max 27.478 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1411 _reflns_number_gt 1353 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.631 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _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 1.171.39.9g (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)' _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^)+(0.0348P)^2^+0.0893P] 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 1411 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _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 O1 O 0.51320(17) 0.52506(16) 0.61760(4) 0.0134(2) Uani 1 1 d . . . . . O52 O 0.6582(2) 0.09633(18) 0.73092(5) 0.0196(2) Uani 1 1 d . . . . . O53 O 0.32506(19) 0.13458(18) 0.67096(5) 0.0198(2) Uani 1 1 d . . . . . O23 O 0.90463(19) 1.09197(19) 0.54507(5) 0.0198(2) Uani 1 1 d . . . . . H23 H 0.967(4) 1.203(4) 0.5204(9) 0.042(6) Uiso 1 1 d . . . . . N51 N 0.5342(2) 0.1998(2) 0.68982(5) 0.0143(2) Uani 1 1 d . . . . . N22 N 0.6556(2) 1.05505(19) 0.52528(5) 0.0162(2) Uani 1 1 d . . . . . C5 C 0.6473(3) 0.4102(2) 0.66274(5) 0.0128(2) Uani 1 1 d . . . . . C2 C 0.6651(3) 0.7172(2) 0.59985(6) 0.0133(3) Uani 1 1 d . . . . . C4 C 0.8730(2) 0.5146(2) 0.67525(6) 0.0152(3) Uani 1 1 d . . . . . H4 H 0.996184 0.464065 0.705198 0.018 Uiso 1 1 calc R U . . . C21 C 0.5520(3) 0.8738(2) 0.55290(6) 0.0149(3) Uani 1 1 d . . . . . H21 H 0.381980 0.838375 0.541264 0.018 Uiso 1 1 calc R U . . . C3 C 0.8864(2) 0.7163(2) 0.63397(6) 0.0153(3) Uani 1 1 d . . . . . H3 H 1.022043 0.828841 0.630580 0.018 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 O1 0.0124(4) 0.0128(4) 0.0148(4) 0.0020(3) -0.0017(3) -0.0010(4) O52 0.0195(5) 0.0187(4) 0.0205(4) 0.0075(4) -0.0002(4) 0.0027(4) O53 0.0161(4) 0.0176(5) 0.0256(5) 0.0004(4) -0.0014(4) -0.0046(4) O23 0.0180(5) 0.0186(5) 0.0228(5) 0.0064(4) -0.0015(4) -0.0047(4) N51 0.0142(5) 0.0127(5) 0.0161(5) -0.0004(4) 0.0017(4) 0.0004(4) N22 0.0173(5) 0.0153(6) 0.0162(5) 0.0006(4) -0.0004(4) 0.0023(5) C5 0.0137(5) 0.0119(5) 0.0127(5) 0.0010(4) 0.0009(5) 0.0016(5) C2 0.0144(6) 0.0108(5) 0.0149(5) -0.0006(4) 0.0021(5) -0.0017(5) C4 0.0137(6) 0.0153(6) 0.0166(6) 0.0006(5) -0.0006(5) 0.0000(5) C21 0.0147(6) 0.0153(6) 0.0146(5) -0.0003(5) -0.0015(5) 0.0017(5) C3 0.0129(6) 0.0154(6) 0.0176(6) 0.0003(5) 0.0012(5) -0.0016(5) _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 O1 C5 1.3482(15) . ? O1 C2 1.3810(16) . ? O52 N51 1.2298(15) . ? O53 N51 1.2265(15) . ? O23 N22 1.3933(15) . ? O23 H23 0.87(2) . ? N51 C5 1.4262(17) . ? N22 C21 1.2811(18) . ? C5 C4 1.3485(18) . ? C2 C3 1.3724(19) . ? C2 C21 1.4472(18) . ? C4 C3 1.4180(18) . ? C4 H4 0.9500 . ? C21 H21 0.9500 . ? C3 H3 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 C5 O1 C2 104.51(10) . . ? N22 O23 H23 106.1(14) . . ? O53 N51 O52 124.92(11) . . ? O53 N51 C5 118.90(11) . . ? O52 N51 C5 116.18(11) . . ? C21 N22 O23 112.20(11) . . ? O1 C5 C4 113.65(11) . . ? O1 C5 N51 116.73(11) . . ? C4 C5 N51 129.62(12) . . ? C3 C2 O1 110.28(11) . . ? C3 C2 C21 135.62(13) . . ? O1 C2 C21 114.04(11) . . ? C5 C4 C3 104.95(11) . . ? C5 C4 H4 127.5 . . ? C3 C4 H4 127.5 . . ? N22 C21 C2 127.27(13) . . ? N22 C21 H21 116.4 . . ? C2 C21 H21 116.4 . . ? C2 C3 C4 106.61(12) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? 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 C2 O1 C5 C4 0.12(14) . . . . ? C2 O1 C5 N51 -179.64(10) . . . . ? O53 N51 C5 O1 0.20(17) . . . . ? O52 N51 C5 O1 179.94(10) . . . . ? O53 N51 C5 C4 -179.50(13) . . . . ? O52 N51 C5 C4 0.2(2) . . . . ? C5 O1 C2 C3 0.03(13) . . . . ? C5 O1 C2 C21 -177.48(10) . . . . ? O1 C5 C4 C3 -0.21(15) . . . . ? N51 C5 C4 C3 179.50(12) . . . . ? O23 N22 C21 C2 0.36(18) . . . . ? C3 C2 C21 N22 8.0(2) . . . . ? O1 C2 C21 N22 -175.29(12) . . . . ? O1 C2 C3 C4 -0.16(15) . . . . ? C21 C2 C3 C4 176.60(14) . . . . ? C5 C4 C3 C2 0.22(14) . . . . ? 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 O23 H23 N22 0.87(2) 1.93(2) 2.7876(15) 170(2) 4_576 yes C4 H4 O52 0.95 2.38 3.2044(17) 144.3 3_756 yes C4 H4 O53 0.95 2.62 3.1759(16) 118.1 1_655 yes C3 H3 O53 0.95 2.48 3.3605(17) 154.8 1_665 yes _refine_diff_density_max 0.185 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.035 _shelx_res_file ; TITL 2017ncs0557z_a.res in P2(1)2(1)2(1) 557z.res created by SHELXL-2017/1 at 09:06:28 on 04-Oct-2017 REM Old TITL 2017ncs0557z in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.060, Rweak 0.018, Alpha 0.000, Orientation as input REM Flack x = 0.252 ( 0.264 ) from Parsons' quotients REM Formula found by SHELXT: C6 N O4 CELL 0.71075 5.2711 5.5198 21.2019 90 90 90 ZERR 4 0.0002 0.0002 0.0007 0 0 0 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 UNIT 20 16 8 16 SIZE 0.08 0.07 0.03 TEMP -173 L.S. 10 PLAN 20 BOND $H CONF HTAB EQIV $1 x+1/2, -y+5/2, -z+1 HTAB O23 N22_$1 EQIV $2 -x+2, y+1/2, -z+3/2 HTAB C4 O52_$2 EQIV $3 x+1, y, z HTAB C4 O53_$3 EQIV $4 x+1, y+1, z HTAB C3 O53_$4 LIST 4 FMAP 2 ACTA twin WGHT 0.034800 0.089300 FVAR 1.15087 O1 4 0.513204 0.525057 0.617596 11.00000 0.01242 0.01280 = 0.01483 0.00202 -0.00165 -0.00096 O52 4 0.658162 0.096332 0.730918 11.00000 0.01946 0.01873 = 0.02052 0.00753 -0.00021 0.00270 O53 4 0.325056 0.134583 0.670959 11.00000 0.01614 0.01756 = 0.02562 0.00035 -0.00144 -0.00460 O23 4 0.904630 1.091974 0.545075 11.00000 0.01803 0.01865 = 0.02284 0.00638 -0.00145 -0.00474 H23 2 0.966921 1.202794 0.520446 11.00000 0.04191 N51 3 0.534158 0.199772 0.689823 11.00000 0.01420 0.01271 = 0.01608 -0.00044 0.00168 0.00043 N22 3 0.655557 1.055053 0.525279 11.00000 0.01727 0.01530 = 0.01615 0.00057 -0.00042 0.00230 C5 1 0.647258 0.410190 0.662745 11.00000 0.01365 0.01191 = 0.01275 0.00103 0.00087 0.00163 C2 1 0.665123 0.717155 0.599852 11.00000 0.01442 0.01075 = 0.01487 -0.00063 0.00211 -0.00173 C4 1 0.872995 0.514602 0.675255 11.00000 0.01369 0.01531 = 0.01664 0.00063 -0.00065 0.00003 AFIX 43 H4 2 0.996184 0.464065 0.705198 11.00000 -1.20000 AFIX 0 C21 1 0.552013 0.873850 0.552901 11.00000 0.01471 0.01532 = 0.01460 -0.00034 -0.00151 0.00174 AFIX 43 H21 2 0.381980 0.838375 0.541264 11.00000 -1.20000 AFIX 0 C3 1 0.886382 0.716284 0.633966 11.00000 0.01290 0.01536 = 0.01759 0.00027 0.00118 -0.00155 AFIX 43 H3 2 1.022043 0.828841 0.630580 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2017ncs0557z_a.res in P2(1)2(1)2(1) REM R1 = 0.0211 for 1353 Fo > 4sig(Fo) and 0.0223 for all 1411 data REM 104 parameters refined using 0 restraints END WGHT 0.0325 0.0952 REM Instructions for potential hydrogen bonds HTAB O23 N22_$1 HTAB C4 O52_$2 HTAB C4 O53_$3 HTAB C3 O53_$4 REM Highest difference peak 0.185, deepest hole -0.177, 1-sigma level 0.035 Q1 1 0.8620 0.6316 0.6652 11.00000 0.05 0.18 Q2 1 0.6253 0.8031 0.5777 11.00000 0.05 0.18 Q3 1 0.7933 0.4117 0.6626 11.00000 0.05 0.17 Q4 1 0.7626 0.7460 0.6219 11.00000 0.05 0.16 Q5 1 0.6048 0.3184 0.6748 11.00000 0.05 0.14 Q6 1 0.8019 0.7075 0.6077 11.00000 0.05 0.14 Q7 1 0.7409 0.4783 0.6808 11.00000 0.05 0.13 Q8 1 0.6490 0.8993 0.5306 11.00000 0.05 0.11 Q9 1 0.5965 0.4450 0.6415 11.00000 0.05 0.11 Q10 1 0.8414 1.1552 0.5874 11.00000 0.05 0.10 Q11 1 0.2762 0.2670 0.6479 11.00000 0.05 0.10 Q12 1 0.5815 1.0153 0.5668 11.00000 0.05 0.10 Q13 1 0.6291 0.3925 0.7614 11.00000 0.05 0.10 Q14 1 1.2650 0.7219 0.6177 11.00000 0.05 0.09 Q15 1 0.5876 0.6332 0.6089 11.00000 0.05 0.09 Q16 1 1.1267 1.3755 0.5542 11.00000 0.05 0.09 Q17 1 0.6620 0.9132 0.6578 11.00000 0.05 0.09 Q18 1 0.6309 1.2374 0.5744 11.00000 0.05 0.09 Q19 1 0.3930 0.2899 0.7526 11.00000 0.05 0.09 Q20 1 0.8402 0.6597 0.7399 11.00000 0.05 0.08 ; _shelx_res_checksum 71873 _shelx_hkl_file ; 0 0 2 130.20 2.60 0 0 -2 128.85 2.80 0 0 -3 0.25 0.60 0 0 3 0.33 0.36 0 0 3 0.12 0.55 0 0 -3 -0.17 0.36 0 0 4 999.02 19.11 0 0 -4 998.63 19.06 0 0 -4 1004.11 18.65 0 0 4 1005.35 18.65 0 0 5 0.08 0.54 0 0 -5 -0.53 0.78 0 0 5 0.20 0.86 0 0 -5 -0.51 0.57 0 0 6 2268.11 42.84 0 0 -6 2313.19 42.76 0 0 6 2290.35 42.13 0 0 -6 2275.61 42.13 0 0 7 -0.76 1.03 0 0 -7 -0.09 0.67 0 0 -7 -0.16 0.85 0 0 7 -0.29 0.58 0 0 8 430.35 9.76 0 0 -8 445.07 9.58 0 0 -8 443.11 8.88 0 0 8 427.58 8.85 0 0 -9 0.40 1.00 0 0 9 0.26 0.68 0 0 -9 0.04 0.82 0 0 9 -0.08 1.23 0 0 -10 719.36 14.63 0 0 10 679.94 14.85 0 0 10 679.99 13.67 0 0 -10 684.63 13.67 0 0 -11 0.08 1.07 0 0 11 0.76 1.48 0 0 11 0.09 0.82 0 0 12 292.44 6.74 0 0 12 297.31 8.04 0 0 -12 301.94 7.61 0 0 -13 0.64 1.13 0 0 13 0.57 1.56 0 0 13 0.16 0.79 0 0 -14 2806.83 54.80 0 0 14 2891.74 55.58 0 0 14 2897.24 53.69 0 0 -15 0.51 1.19 0 0 15 -0.31 0.97 0 0 15 -0.79 1.80 0 0 16 3.36 1.80 0 0 16 4.29 1.07 0 0 -16 7.02 1.44 0 0 17 0.57 1.10 0 0 17 -0.89 1.87 0 0 -17 1.02 1.28 0 0 18 485.29 10.87 0 0 18 475.79 12.78 0 0 -18 482.76 11.90 0 0 19 0.64 1.24 0 0 -19 0.49 1.35 0 0 -19 -0.99 1.53 0 0 19 1.00 2.06 0 0 20 177.14 5.33 0 0 -20 185.57 6.24 0 0 -21 0.76 1.02 0 0 -21 0.14 1.56 0 0 21 -1.66 1.40 0 0 -22 119.13 5.14 0 0 22 121.60 4.39 0 0 23 -1.45 1.27 0 0 -23 0.56 1.08 0 0 -23 -0.44 1.67 0 0 -24 0.60 1.73 0 0 24 1.81 1.43 0 0 -24 0.67 1.17 0 0 25 1.47 1.49 0 0 -25 -0.47 1.74 0 0 -26 19.01 2.54 0 0 -26 17.25 1.71 0 0 26 21.29 2.21 0 0 -27 -0.99 1.85 0 0 -27 1.33 1.25 0 0 27 -0.45 1.57 0 1 0 0.23 0.41 0 -1 0 0.28 0.71 0 1 0 0.27 0.73 0 -1 0 0.15 0.38 0 1 1 1.04 0.31 0 -1 1 1.05 0.51 0 1 -1 1.04 0.52 0 -1 1 2.03 0.79 0 1 -1 0.96 0.73 0 -1 1 1.57 0.40 0 -1 -1 1.57 0.77 0 1 1 1.16 0.39 0 1 1 0.90 0.72 0 -1 2 154.37 3.64 0 -1 2 169.52 3.72 0 -1 -2 157.95 3.27 0 1 -2 158.59 3.36 0 1 2 159.69 3.56 0 1 2 159.65 3.27 0 1 -2 161.69 3.75 0 1 2 157.80 3.15 0 -1 2 162.85 3.38 0 1 -2 164.40 3.78 0 -1 -2 166.37 3.67 0 1 3 444.13 8.44 0 1 -3 466.03 8.75 0 1 3 447.03 8.65 0 1 -3 455.21 9.02 0 -1 3 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479.60 10.43 -2 3 12 474.88 9.46 -2 3 12 493.38 11.22 2 3 -12 466.29 13.24 2 -3 12 484.35 11.79 -2 3 11 28.43 1.11 2 3 -11 28.91 2.38 2 3 -11 28.13 3.01 2 -3 11 28.86 1.74 -2 -3 -11 28.07 1.63 -2 3 11 30.32 1.17 -2 3 11 31.18 2.08 2 -3 11 30.68 2.44 2 3 -10 237.65 6.77 2 -3 10 239.65 5.67 -2 -3 -10 230.75 5.59 -2 3 10 232.37 5.03 -2 3 10 228.83 4.75 -2 3 10 235.12 6.10 2 3 -10 244.68 8.15 2 -3 10 240.21 6.73 -2 3 9 43.40 1.64 2 3 -9 45.69 2.78 2 -3 9 46.05 1.94 -2 -3 -9 47.73 2.00 2 3 -9 43.56 3.39 -2 3 9 50.85 2.25 2 -3 9 43.69 2.57 -2 3 8 269.40 5.76 -2 -3 -8 259.37 7.27 2 3 -8 283.22 7.19 2 -3 8 274.35 5.89 -2 -3 -8 279.22 6.01 2 3 -8 268.08 8.34 -2 3 8 284.90 6.11 2 -3 8 278.11 6.77 2 3 -7 375.49 9.24 -2 -3 -7 383.08 9.60 2 -3 7 380.58 8.05 -2 3 7 376.92 8.20 -2 -3 -7 383.43 8.24 -2 3 7 373.80 7.97 2 3 -7 389.84 10.61 2 -3 7 382.57 8.77 2 3 -6 30.26 2.26 -2 3 6 31.18 1.70 2 -3 6 32.17 1.41 -2 -3 -6 30.91 2.33 -2 3 6 27.59 1.14 2 3 -6 31.33 2.75 -2 -3 -6 28.64 1.56 2 -3 6 31.24 1.75 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9 41.47 2.67 2 -3 -9 45.33 1.78 -2 3 -9 45.89 2.00 2 -3 -9 51.68 1.73 2 3 9 46.34 2.31 2 3 9 40.56 2.25 2 3 9 43.27 2.56 -2 3 -9 44.41 2.59 2 3 9 47.88 2.23 -2 3 -9 44.18 2.01 -2 -3 10 237.07 6.74 2 -3 -10 234.27 5.35 -2 3 -10 239.91 5.91 -2 3 -10 232.41 6.54 2 3 10 241.46 5.96 2 3 10 241.53 6.18 2 -3 -10 239.95 5.45 2 3 10 228.03 6.23 2 3 10 230.65 6.61 -2 3 -10 241.18 5.82 2 3 11 29.19 1.99 2 -3 -11 31.24 1.42 -2 -3 11 28.71 2.27 -2 3 -11 28.41 1.79 2 -3 -11 31.18 1.56 2 3 11 31.92 2.08 -2 3 -11 25.49 2.17 2 3 11 27.57 2.23 -2 3 -11 31.32 1.87 2 3 11 27.03 1.80 2 3 12 492.15 10.91 2 -3 -12 482.64 9.83 -2 3 -12 491.65 10.84 -2 3 -12 486.71 11.37 -2 -3 12 494.50 11.34 2 3 12 478.15 11.14 2 -3 -12 478.16 10.31 2 3 12 492.75 11.51 -2 3 -12 480.25 10.59 2 3 13 528.54 11.58 2 -3 -13 516.09 10.42 -2 3 -13 522.24 11.64 -2 3 -13 507.80 12.05 -2 -3 13 515.89 11.79 2 -3 -13 516.52 11.12 2 3 13 529.15 12.22 -2 3 -13 522.77 11.38 2 3 13 513.59 11.97 2 3 14 250.66 6.53 2 -3 -14 237.67 5.40 -2 3 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11 83.78 3.14 2 4 -11 78.66 4.93 -2 4 10 418.01 8.79 2 4 -10 407.49 10.50 2 -4 10 410.08 8.88 -2 4 10 400.57 8.27 -2 -4 -10 391.07 8.82 2 -4 10 404.25 9.75 -2 4 10 407.55 8.99 2 4 -10 404.23 11.98 -2 4 9 26.47 1.67 2 4 -9 25.43 2.48 -2 4 9 22.69 1.10 -2 -4 -9 24.45 1.58 2 -4 9 27.10 1.54 2 -4 9 23.31 1.85 -2 4 9 25.79 1.46 2 4 -9 20.41 2.89 -2 4 8 76.46 2.79 2 4 -8 81.02 3.78 2 -4 8 75.44 2.46 -2 4 8 64.17 1.81 -2 -4 -8 73.19 2.59 2 -4 8 76.49 2.88 -2 4 8 67.84 2.10 2 4 -8 75.68 4.64 -2 4 7 110.01 3.62 2 4 -7 100.78 4.34 2 -4 7 102.00 2.97 2 -4 7 107.47 3.31 -2 -4 -7 108.56 3.28 2 4 -7 106.81 5.18 -2 4 6 61.07 2.76 2 4 -6 54.14 3.20 -2 -4 -6 58.83 3.73 2 -4 6 56.97 1.97 2 -4 6 56.04 2.05 2 4 -6 56.18 3.81 -2 -4 -6 61.46 2.37 -2 4 5 51.62 2.65 -2 -4 -5 50.10 3.48 2 -4 5 53.87 1.80 2 -4 5 50.63 1.67 2 4 -5 56.58 3.75 -2 -4 -5 53.23 2.21 -2 4 4 83.75 3.34 2 -4 4 85.99 2.16 2 4 -4 74.17 4.10 -2 -4 -4 80.55 4.19 -2 -4 -4 81.23 2.71 -2 -4 -3 287.90 6.76 -2 -4 -3 298.80 8.84 -2 4 3 289.49 7.62 2 4 -3 296.94 8.73 2 -4 3 287.96 5.93 -2 -4 -2 257.66 8.23 -2 4 2 267.06 7.29 -2 -4 -2 286.33 6.55 2 -4 2 293.37 7.01 -2 -4 -2 272.84 6.87 2 4 -2 285.57 8.20 2 -4 2 260.47 5.43 -2 -4 -1 18.27 1.58 2 -4 1 20.01 1.64 2 4 -1 19.43 2.05 -2 -4 -1 15.41 2.41 -2 4 1 18.23 1.99 -2 -4 -1 20.71 1.78 2 4 -1 16.60 2.15 -2 -4 0 135.42 5.53 -2 4 0 140.50 4.88 2 -4 0 145.85 4.30 -2 -4 0 138.68 4.15 -2 -4 0 139.03 4.44 2 4 0 137.74 5.13 2 4 0 131.51 4.64 -2 -4 1 18.69 1.66 2 -4 -1 17.40 1.59 2 4 1 16.44 1.93 -2 -4 1 16.00 2.44 -2 4 -1 15.84 1.97 -2 -4 1 20.99 1.85 2 4 1 17.45 2.05 2 4 2 266.32 7.13 -2 -4 2 270.35 8.31 -2 4 -2 277.04 7.60 2 -4 -2 265.78 6.68 -2 -4 2 265.06 7.00 2 4 2 274.21 7.64 -2 -4 2 268.38 6.74 2 4 3 285.25 7.41 -2 -4 3 279.22 8.52 -2 4 -3 292.37 7.93 2 -4 -3 278.99 6.95 -2 -4 3 281.65 7.37 2 4 3 286.33 7.89 -2 4 -3 291.46 5.93 -2 -4 3 275.74 6.98 2 4 4 76.74 3.28 -2 -4 4 80.70 4.22 -2 4 -4 83.44 3.80 2 -4 -4 79.46 2.99 -2 -4 4 92.96 3.58 2 4 4 86.28 3.05 2 4 4 85.65 3.71 -2 4 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4.18 -5 3 7 -0.05 1.00 5 -3 7 1.00 1.09 -5 -3 -7 0.16 2.05 5 -3 7 0.56 1.06 5 -3 7 0.97 1.40 5 3 -7 -1.39 2.58 5 -3 6 33.25 1.93 -5 -3 -6 27.19 2.98 5 -3 6 28.52 2.16 5 -3 6 29.62 1.87 5 3 -6 30.49 3.69 -5 3 6 30.23 1.24 5 -3 5 62.33 2.53 -5 -3 -5 58.82 3.97 5 -3 5 59.69 2.53 5 -3 5 62.09 2.94 5 3 -5 54.45 4.51 5 -3 4 67.55 2.50 -5 -3 -4 62.41 4.15 5 -3 4 70.67 2.70 5 3 -4 59.96 4.50 5 -3 4 67.62 3.01 -5 -3 -3 130.43 5.70 5 -3 3 135.59 3.68 5 -3 3 129.64 3.91 5 3 -3 114.40 6.03 5 -3 3 130.49 4.30 -5 -3 -2 61.12 4.12 5 -3 2 59.66 2.10 -5 3 2 60.74 2.78 -5 3 2 57.87 2.12 5 3 -2 58.20 4.40 5 -3 2 58.88 2.41 -5 -3 -1 268.07 8.79 5 -3 1 286.57 6.15 -5 3 1 279.49 7.12 -5 3 1 279.39 6.29 5 3 -1 273.19 9.38 -5 -3 0 265.14 8.76 5 -3 0 282.18 5.98 -5 3 0 280.76 7.15 -5 3 0 277.37 6.28 5 3 0 287.02 9.41 5 -3 0 271.98 6.54 -5 -3 1 262.16 8.70 5 -3 -1 278.61 5.90 -5 3 -1 283.01 7.22 -5 3 -1 286.45 6.39 5 3 1 286.57 9.29 5 -3 -1 274.63 6.51 -5 -3 2 59.34 3.91 5 -3 -2 58.18 1.74 -5 3 -2 59.84 2.83 -5 3 -2 57.08 2.23 5 3 2 59.27 4.08 -5 -3 3 123.58 5.54 -5 3 -3 124.98 4.25 -5 3 -3 124.23 3.55 5 -3 -3 122.08 2.92 5 3 3 121.18 5.64 -5 -3 4 62.30 3.99 -5 3 -4 59.89 2.35 5 -3 -4 57.36 1.68 5 3 4 56.10 3.98 -5 -3 5 50.36 3.63 -5 3 -5 59.54 2.36 5 -3 -5 54.98 1.65 5 3 5 58.00 3.98 -5 3 -6 30.98 1.81 -5 -3 6 28.38 2.98 5 -3 -6 27.75 1.13 5 3 6 28.40 3.09 5 -3 -7 -0.06 0.85 -5 -3 7 -0.73 1.94 5 -3 -7 0.34 0.49 5 3 7 -0.17 2.01 -5 3 -7 -0.30 1.08 5 -3 -8 40.97 2.02 -5 -3 8 39.32 3.17 5 3 8 38.64 3.38 5 3 8 36.98 3.11 -5 -3 9 52.23 3.57 5 3 9 58.68 3.99 5 3 9 56.17 3.63 5 -3 -10 28.29 1.83 -5 -3 10 20.75 2.58 5 3 10 23.12 2.73 5 3 10 26.94 3.06 5 -3 -11 49.89 2.46 -5 -3 11 40.75 3.04 5 3 11 46.89 3.74 -5 -3 11 52.05 3.52 5 3 11 45.52 3.37 5 -3 -12 45.75 2.43 -5 -3 12 43.55 2.99 5 3 12 41.11 3.59 -5 -3 12 45.57 3.39 5 -3 -13 44.89 2.45 -5 -3 13 37.83 2.74 5 3 13 41.84 3.58 -5 -3 13 39.04 3.27 5 3 13 37.75 3.32 5 -3 -14 19.53 1.85 5 3 14 15.25 2.47 5 3 14 16.70 2.94 -5 -4 -10 65.27 4.61 5 -4 10 64.48 3.11 5 -4 10 62.40 2.46 5 4 -10 62.04 5.42 -5 -4 -9 3.00 2.60 5 -4 9 4.38 1.45 5 4 -9 3.30 3.24 -5 -4 -8 44.79 4.03 5 4 -8 32.06 4.34 -5 -4 -7 82.14 5.06 5 -4 7 90.05 3.36 5 4 -7 86.30 5.79 -5 -4 -6 9.57 2.87 5 -4 6 13.61 1.66 5 4 -6 11.18 3.20 -5 -4 -5 282.55 9.68 5 -4 5 283.38 7.10 -5 -4 -4 41.11 3.97 5 4 -4 36.34 4.16 5 -4 4 44.36 2.31 -5 -4 -3 33.60 3.60 5 4 -3 31.89 3.94 -5 -4 -2 71.05 4.93 5 4 -2 70.35 5.03 -5 -4 -1 17.79 3.23 5 4 -1 14.70 3.11 -5 -4 0 0.38 2.54 5 4 0 2.30 2.38 -5 -4 1 19.87 3.16 5 4 1 13.90 2.89 -5 -4 2 74.88 4.87 5 4 2 76.55 4.89 -5 -4 3 26.59 3.42 5 4 3 29.91 3.38 -5 -4 4 52.39 4.17 5 4 4 45.98 4.03 -5 -4 5 271.63 9.16 5 4 5 271.11 9.32 -5 -4 6 8.47 2.54 5 4 6 9.54 2.78 -5 -4 7 84.43 4.88 5 4 7 87.23 5.07 -5 -4 8 39.04 3.48 5 4 8 35.41 3.61 -5 -4 9 0.50 2.19 -5 -4 10 61.32 4.04 5 4 10 58.53 4.31 -6 0 0 552.95 12.46 6 0 0 536.28 14.06 -6 0 -1 127.88 4.47 -6 0 1 119.29 4.31 6 0 1 115.31 5.30 6 0 -1 125.98 5.69 -6 0 -2 111.29 4.23 -6 0 2 108.91 4.10 6 0 2 121.68 5.30 6 0 -2 120.70 5.68 -6 0 -3 54.64 2.99 6 0 3 55.31 3.74 6 0 -3 55.73 4.05 -6 0 -4 38.86 2.57 -6 0 4 40.35 2.49 6 0 4 41.56 3.26 6 0 -4 41.10 3.71 -6 0 -5 2.59 1.42 6 0 5 2.48 1.87 -6 0 5 -0.41 1.38 6 0 5 3.04 1.96 6 0 -5 1.69 2.27 -6 0 -6 15.39 2.00 -6 0 6 17.92 1.82 6 0 6 14.76 2.36 6 0 6 16.26 2.38 6 0 -6 18.21 3.14 -6 0 -7 10.00 1.82 -6 0 7 6.74 1.41 6 0 7 5.99 1.95 6 0 7 6.67 2.17 6 0 -7 9.57 2.91 6 0 8 48.79 3.49 6 0 8 52.85 3.54 6 0 -8 63.96 4.71 -6 0 -8 58.47 3.18 -6 0 -9 20.77 2.25 6 0 9 19.76 2.55 6 0 9 23.23 2.76 6 0 -9 27.60 3.53 6 0 10 92.00 4.68 6 0 10 94.42 4.61 6 0 -10 104.97 5.90 -6 0 -10 94.92 4.17 6 0 -11 10.45 3.03 6 0 11 8.61 2.30 -6 0 -11 10.40 1.95 6 0 11 12.34 2.44 6 0 12 119.68 5.38 6 0 12 115.90 5.25 -6 0 12 125.67 5.05 6 0 -12 126.36 6.75 -6 0 -12 127.22 4.93 6 0 13 207.68 7.16 6 0 13 194.90 7.09 -6 0 13 202.36 6.63 6 0 -13 210.51 8.75 -6 0 -13 193.51 6.51 6 1 -12 2.57 2.99 -6 1 12 -0.55 1.68 -6 -1 -12 1.10 1.91 6 -1 12 1.76 1.95 -6 -1 -11 32.52 2.97 6 -1 11 34.84 2.99 -6 1 11 32.15 2.59 6 -1 11 32.32 2.92 6 1 -11 29.70 4.02 -6 -1 -10 99.20 4.49 6 -1 10 97.33 4.52 6 -1 10 93.67 4.51 6 1 -10 94.45 6.03 -6 -1 -9 39.44 3.06 6 -1 9 43.32 3.22 6 -1 9 43.28 3.16 6 1 -9 40.43 4.36 -6 -1 -8 32.32 2.84 6 -1 8 33.82 2.85 6 -1 8 33.83 2.91 6 -1 7 31.28 2.79 -6 -1 -7 24.36 2.58 6 -1 7 35.50 2.87 6 1 -7 29.03 3.68 -6 -1 -6 51.30 3.23 6 -1 6 51.69 3.40 6 1 -6 50.45 4.43 6 -1 6 55.73 3.36 -6 -1 -5 162.56 5.74 -6 1 5 156.06 4.47 6 -1 5 169.23 5.96 6 1 -5 162.51 7.10 6 -1 5 160.85 5.80 -6 -1 -4 84.68 3.92 -6 1 4 80.35 3.03 6 -1 4 80.45 4.14 6 1 -4 87.78 5.29 -6 1 3 58.67 2.64 -6 -1 -3 60.81 3.47 6 -1 3 61.46 2.76 6 -1 3 64.92 3.69 6 1 -3 58.84 4.32 -6 1 2 43.31 2.29 -6 -1 -2 44.60 3.06 6 -1 2 42.56 2.26 6 -1 2 48.01 3.22 6 1 -2 40.80 3.82 -6 1 1 21.88 1.80 -6 -1 -1 16.28 2.15 6 -1 1 19.05 1.62 6 -1 1 22.87 2.65 6 1 -1 18.56 2.81 -6 -1 0 49.49 3.16 6 -1 0 53.05 2.44 6 1 0 48.28 3.83 6 -1 0 53.84 3.52 -6 1 0 47.51 2.48 -6 1 -1 20.68 1.82 6 -1 -1 18.99 1.60 6 1 1 20.98 3.00 6 -1 -1 24.56 2.77 -6 -1 2 43.30 3.00 6 -1 -2 46.37 2.29 6 1 2 48.84 3.75 6 -1 -2 46.44 3.48 -6 1 -2 40.07 2.35 -6 -1 3 61.89 3.44 6 1 3 59.10 4.09 6 -1 -3 65.60 4.06 -6 1 -3 66.17 2.94 -6 -1 4 83.40 3.92 6 1 4 85.32 4.63 6 -1 -4 86.52 4.68 -6 1 -4 84.74 3.41 -6 -1 5 159.10 5.47 6 1 5 152.70 6.26 6 -1 -5 166.44 6.59 -6 1 -5 154.83 4.95 -6 -1 6 51.93 3.07 6 1 6 49.85 3.70 6 -1 -6 46.36 3.83 -6 1 -6 52.38 2.74 -6 -1 7 30.12 2.43 6 1 7 30.00 3.19 -6 1 -7 30.60 2.25 6 -1 -7 27.61 3.34 -6 -1 8 29.64 2.31 6 1 8 31.81 3.18 -6 1 -8 28.94 2.26 6 -1 -9 40.86 3.76 6 1 9 41.89 3.54 -6 1 -9 39.31 2.58 6 1 10 101.49 5.00 6 -1 -10 98.35 5.41 -6 1 -10 91.32 3.94 6 -1 -11 36.62 3.81 6 1 11 27.18 3.13 -6 1 -11 30.78 2.50 -6 1 -12 -0.65 1.54 6 1 12 0.33 2.24 -6 -1 12 1.25 1.95 -6 2 10 14.42 1.85 6 -2 10 11.14 2.14 -6 -2 -10 15.29 2.78 6 2 -10 13.22 3.68 6 -2 9 5.82 2.08 -6 -2 -9 4.52 2.26 6 -2 9 5.58 1.79 6 2 -9 3.90 2.90 -6 2 9 4.14 1.51 -6 -2 -8 79.37 4.44 6 -2 8 82.67 4.03 6 2 -8 73.67 5.52 -6 -2 -7 10.62 2.38 6 -2 7 8.31 1.54 6 -2 7 10.82 1.98 6 2 -7 5.81 2.93 6 -2 7 7.11 2.00 6 -2 6 37.38 2.27 -6 -2 -6 35.32 3.23 6 -2 6 38.76 2.71 6 -2 6 35.90 2.82 6 2 -6 39.18 4.18 -6 -2 -5 16.68 2.54 6 -2 5 13.21 1.48 6 -2 5 11.84 2.05 6 -2 5 14.16 1.95 6 2 -5 11.01 3.08 -6 -2 -4 48.54 3.59 6 -2 4 53.29 2.50 6 -2 4 57.00 3.17 6 2 -4 58.93 4.60 -6 2 3 11.05 1.31 -6 -2 -3 16.19 2.55 6 -2 3 11.65 1.37 6 -2 3 13.52 2.01 6 2 -3 13.12 2.98 6 -2 2 24.07 1.70 -6 -2 -2 23.43 2.83 6 2 -2 26.95 3.47 -6 2 2 21.86 1.60 -6 -2 -1 84.49 4.50 6 -2 1 80.46 2.94 6 2 -1 75.04 4.89 -6 2 1 83.98 2.96 -6 -2 0 35.28 3.09 6 -2 0 34.51 1.83 6 -2 0 34.32 2.77 6 2 0 31.67 3.55 -6 2 0 36.08 1.97 -6 -2 1 80.28 4.29 6 -2 -1 81.29 2.85 6 2 1 76.71 4.98 6 -2 -1 77.97 3.90 -6 2 -1 82.87 3.07 -6 -2 2 25.79 2.88 6 -2 -2 24.70 1.54 6 2 2 27.74 3.26 6 -2 -2 22.08 2.48 -6 2 -2 20.62 1.74 -6 2 -3 10.66 1.51 -6 -2 3 11.52 2.38 6 -2 -3 12.01 1.23 6 2 3 10.21 2.75 6 -2 -3 12.67 2.17 -6 -2 4 54.29 3.67 6 -2 -4 54.77 2.24 6 2 4 59.05 4.22 -6 2 -4 59.82 2.74 6 -2 -5 6.72 2.01 -6 2 -5 10.57 1.58 -6 -2 5 12.59 2.41 6 -2 -5 11.63 1.23 6 2 5 6.90 2.48 -6 -2 6 34.67 2.93 6 2 6 34.66 3.41 6 -2 -6 37.32 3.05 -6 2 -6 36.37 2.31 6 -2 -7 8.01 2.17 -6 2 -7 9.69 1.65 -6 -2 7 6.33 2.05 6 2 7 9.75 2.42 -6 -2 8 68.98 3.79 6 2 8 77.06 4.60 6 -2 -8 75.53 4.14 -6 2 -8 73.54 3.29 6 2 8 66.25 4.06 6 -2 -9 2.26 1.82 -6 2 -9 2.74 1.47 -6 -2 9 4.29 1.79 6 2 9 1.98 2.20 6 2 9 3.10 2.15 6 -2 -10 13.31 2.38 -6 2 -10 10.38 1.71 6 2 10 10.16 2.58 6 2 10 13.86 2.62 -6 -3 -6 34.41 3.59 6 -3 6 37.21 2.37 -6 -3 -5 34.17 3.68 6 -3 5 31.93 2.21 6 -3 5 31.16 2.52 -6 -3 -4 85.46 5.03 6 -3 4 83.53 3.39 -6 -3 -3 24.02 3.28 -6 -3 -2 45.08 3.88 6 -3 2 46.74 2.45 -6 -3 -1 74.14 4.66 -6 3 1 77.18 2.78 -6 -3 0 98.58 5.28 -6 3 0 98.01 3.28 -6 -3 1 75.40 4.72 -6 -3 2 41.85 3.77 -6 -3 3 31.09 3.42 -6 -3 4 74.89 4.54 -6 -3 5 24.12 3.13 -6 -3 6 35.83 3.39 0 0 0 0.00 0.00 TITL 2017ncs0557z in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 0.71075 5.271089 5.519823 21.201867 90.0000 90.0000 90.0000 ZERR 3.00 0.000196 0.000208 0.000735 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 15.00 12.00 6.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 61191