data_dm_skp_3_219_autored _audit_creation_date 2021-02-17 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.67(C18 H14 N2 O3)' _chemical_formula_sum 'C12 H9.33 N1.33 O2' _chemical_formula_weight 204.21 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.9733(2) _cell_length_b 15.3701(6) _cell_length_c 19.3784(9) _cell_angle_alpha 90 _cell_angle_beta 92.471(4) _cell_angle_gamma 90 _cell_volume 1479.91(11) _cell_formula_units_Z 6 _cell_measurement_reflns_used 3954 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 24.8970 _cell_measurement_theta_min 1.6820 _shelx_estimated_absorpt_T_max 0.995 _shelx_estimated_absorpt_T_min 0.989 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.72027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1337 _diffrn_reflns_av_unetI/netI 0.1316 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.923 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 66759 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.923 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.802 _diffrn_reflns_theta_min 1.692 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.923 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \f -7.92 176.08 1.00 7.00 15.81 -9.84 -59.25 -- 184 2 \w -100.81 15.19 1.00 7.00 -- -9.84 -59.25 20.08 116 3 \w -26.04 80.96 1.00 7.00 -- -9.90 32.04 -81.82 107 4 \w -100.81 15.19 1.00 7.00 -- -9.84 -59.25 164.08 116 5 \w -100.81 15.19 1.00 7.00 -- -9.84 -59.25 -51.92 116 6 \w -100.81 15.19 1.00 7.00 -- -9.84 -59.25-123.92 116 7 \w -100.81 15.19 1.00 7.00 -- -9.84 -59.25 92.08 116 8 \f -134.27 50.73 1.00 7.00 81.02 -9.84 31.50 -- 185 9 \f -17.73 56.27 1.00 7.00 6.61 -9.84 -31.50 -- 74 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0704644000 _diffrn_orient_matrix_UB_12 0.0255451000 _diffrn_orient_matrix_UB_13 -0.0253296000 _diffrn_orient_matrix_UB_21 0.0739711000 _diffrn_orient_matrix_UB_22 0.0372255000 _diffrn_orient_matrix_UB_23 0.0112115000 _diffrn_orient_matrix_UB_31 0.0997053000 _diffrn_orient_matrix_UB_32 -0.0095954000 _diffrn_orient_matrix_UB_33 -0.0239693000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2689 _reflns_number_total 5498 _reflns_odcompleteness_completeness 92.36 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 33.72 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.316 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.056 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 5498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1927 _refine_ls_R_factor_gt 0.0756 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.2004P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1499 _refine_ls_wR_factor_ref 0.1836 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: N003(H003), C006(H006), C00C(H00C), C00D(H00D), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M) 2.b Idealised Me refined as rotating group: C00N(H00A,H00B,H00E) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 O001 O 0.0423(2) 0.51767(8) 0.36659(7) 0.0389(3) Uani 1 1 d . . . . . O002 O 0.9120(3) 0.05311(10) 0.55522(8) 0.0545(4) Uani 1 1 d . . . . . N003 N -0.3985(3) 0.53398(10) 0.38289(8) 0.0364(4) Uani 1 1 d . . . . . H003 H -0.564319 0.519464 0.370053 0.044 Uiso 1 1 calc R . . . . O004 O 1.1000(3) 0.18013(11) 0.55536(8) 0.0581(5) Uani 1 1 d . . . . . N005 N 0.9310(3) 0.12818(12) 0.53380(8) 0.0405(4) Uani 1 1 d . . . . . C006 C 0.0593(3) 0.32767(11) 0.32985(9) 0.0266(4) Uani 1 1 d . . . . . H006 H 0.119513 0.363908 0.367101 0.032 Uiso 1 1 calc R . . . . C007 C -0.1411(3) 0.35961(11) 0.28197(9) 0.0261(4) Uani 1 1 d . . . . . C008 C 0.1690(3) 0.24611(11) 0.32412(9) 0.0287(4) Uani 1 1 d . . . . . C009 C -0.2729(3) 0.44167(11) 0.28977(9) 0.0270(4) Uani 1 1 d . . . . . C00A C -0.1942(3) 0.50056(11) 0.34901(9) 0.0289(4) Uani 1 1 d . . . . . C00B C -0.2282(3) 0.30434(11) 0.22618(9) 0.0289(4) Uani 1 1 d . . . . . C00C C -0.4366(4) 0.33334(12) 0.17937(9) 0.0336(4) Uani 1 1 d . . . . . H00C H -0.492233 0.297405 0.141504 0.040 Uiso 1 1 calc R . . . . C00D C -0.4775(3) 0.46583(12) 0.24370(9) 0.0316(4) Uani 1 1 d . . . . . H00D H -0.565858 0.519924 0.249678 0.038 Uiso 1 1 calc R . . . . C00E C 0.3679(3) 0.21447(12) 0.37767(9) 0.0309(4) Uani 1 1 d . . . . . C00F C -0.5584(4) 0.41190(12) 0.18781(10) 0.0345(4) Uani 1 1 d . . . . . H00F H -0.697698 0.430252 0.156008 0.041 Uiso 1 1 calc R . . . . C00G C 0.5337(3) 0.27316(12) 0.41542(9) 0.0329(4) Uani 1 1 d . . . . . H00G H 0.518210 0.333676 0.406113 0.039 Uiso 1 1 calc R . . . . C00H C 0.7375(3) 0.15685(13) 0.47919(9) 0.0340(4) Uani 1 1 d . . . . . C00I C -0.1076(4) 0.22140(12) 0.22015(10) 0.0356(4) Uani 1 1 d . . . . . H00I H -0.160362 0.185008 0.182315 0.043 Uiso 1 1 calc R . . . . C00J C 0.7179(3) 0.24493(13) 0.46557(9) 0.0339(4) Uani 1 1 d . . . . . H00J H 0.829622 0.285314 0.490395 0.041 Uiso 1 1 calc R . . . . C00K C 0.0826(4) 0.19271(12) 0.26755(10) 0.0362(4) Uani 1 1 d . . . . . H00K H 0.158331 0.136407 0.262703 0.043 Uiso 1 1 calc R . . . . C00L C 0.5804(4) 0.09682(13) 0.44320(10) 0.0386(5) Uani 1 1 d . . . . . H00L H 0.598489 0.036446 0.452839 0.046 Uiso 1 1 calc R . . . . C00M C 0.3960(4) 0.12582(12) 0.39282(10) 0.0377(4) Uani 1 1 d . . . . . H00M H 0.286462 0.084773 0.368050 0.045 Uiso 1 1 calc R . . . . C00N C -0.3539(4) 0.59358(15) 0.44030(12) 0.0516(6) Uani 1 1 d . . . . . H00A H -0.267643 0.646646 0.424040 0.077 Uiso 1 1 calc GR . . . . H00B H -0.237268 0.565948 0.475975 0.077 Uiso 1 1 calc GR . . . . H00E H -0.526872 0.608419 0.459679 0.077 Uiso 1 1 calc GR . . . . 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 O001 0.0195(6) 0.0398(8) 0.0566(9) -0.0091(6) -0.0065(6) -0.0022(5) O002 0.0677(11) 0.0463(9) 0.0478(9) 0.0045(7) -0.0185(8) 0.0141(8) N003 0.0209(7) 0.0378(9) 0.0500(10) -0.0118(7) -0.0042(7) -0.0009(6) O004 0.0491(9) 0.0679(11) 0.0550(10) 0.0071(8) -0.0234(8) -0.0047(8) N005 0.0401(9) 0.0479(11) 0.0330(9) 0.0025(8) -0.0052(7) 0.0124(8) C006 0.0240(8) 0.0276(9) 0.0277(9) 0.0005(7) -0.0042(7) -0.0008(6) C007 0.0201(8) 0.0279(9) 0.0300(9) 0.0043(7) -0.0020(6) -0.0027(6) C008 0.0259(8) 0.0304(9) 0.0294(9) 0.0019(7) -0.0040(7) 0.0016(7) C009 0.0202(8) 0.0273(9) 0.0332(9) 0.0044(7) -0.0017(7) -0.0033(6) C00A 0.0215(8) 0.0246(9) 0.0401(10) 0.0024(7) -0.0046(7) -0.0004(7) C00B 0.0280(9) 0.0305(9) 0.0277(9) 0.0015(7) -0.0034(7) -0.0020(7) C00C 0.0352(10) 0.0356(10) 0.0290(9) 0.0013(8) -0.0080(8) -0.0028(8) C00D 0.0258(9) 0.0311(9) 0.0373(10) 0.0051(8) -0.0046(7) 0.0000(7) C00E 0.0274(9) 0.0339(10) 0.0310(9) -0.0008(8) -0.0017(7) 0.0051(7) C00F 0.0298(9) 0.0383(11) 0.0345(10) 0.0092(8) -0.0099(7) -0.0022(8) C00G 0.0294(9) 0.0325(10) 0.0366(10) 0.0036(8) -0.0013(8) 0.0010(7) C00H 0.0305(9) 0.0407(11) 0.0301(9) 0.0014(8) -0.0068(7) 0.0083(8) C00I 0.0386(11) 0.0344(10) 0.0331(10) -0.0040(8) -0.0077(8) 0.0015(8) C00J 0.0294(9) 0.0400(11) 0.0322(10) -0.0001(8) -0.0018(7) 0.0002(8) C00K 0.0393(10) 0.0319(10) 0.0368(10) -0.0031(8) -0.0052(8) 0.0064(8) C00L 0.0476(11) 0.0315(10) 0.0356(10) -0.0003(8) -0.0092(9) 0.0120(8) C00M 0.0415(11) 0.0327(10) 0.0379(10) -0.0038(8) -0.0101(8) 0.0052(8) C00N 0.0346(11) 0.0536(14) 0.0660(15) -0.0282(11) -0.0047(10) 0.0033(9) _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 O001 C00A 1.2388(19) . ? O002 N005 1.231(2) . ? N003 C00A 1.336(2) . ? N003 C00N 1.451(3) . ? O004 N005 1.220(2) . ? N005 C00H 1.467(2) . ? C006 C007 1.419(2) . ? C006 C008 1.373(2) . ? C007 C009 1.432(2) . ? C007 C00B 1.428(2) . ? C008 C00E 1.484(2) . ? C008 C00K 1.421(2) . ? C009 C00A 1.501(2) . ? C009 C00D 1.375(2) . ? C00B C00C 1.419(2) . ? C00B C00I 1.416(3) . ? C00C C00F 1.364(3) . ? C00D C00F 1.409(3) . ? C00E C00G 1.406(3) . ? C00E C00M 1.400(3) . ? C00G C00J 1.377(2) . ? C00H C00J 1.382(3) . ? C00H C00L 1.379(3) . ? C00I C00K 1.363(3) . ? C00L C00M 1.384(3) . ? 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 C00A N003 C00N 121.72(15) . . ? O002 N005 C00H 117.86(17) . . ? O004 N005 O002 124.02(17) . . ? O004 N005 C00H 118.12(17) . . ? C008 C006 C007 122.21(16) . . ? C006 C007 C009 123.18(15) . . ? C006 C007 C00B 118.08(15) . . ? C00B C007 C009 118.59(15) . . ? C006 C008 C00E 119.84(16) . . ? C006 C008 C00K 118.79(16) . . ? C00K C008 C00E 121.35(16) . . ? C007 C009 C00A 120.42(15) . . ? C00D C009 C007 119.89(16) . . ? C00D C009 C00A 119.67(16) . . ? O001 C00A N003 121.10(17) . . ? O001 C00A C009 123.48(16) . . ? N003 C00A C009 115.42(15) . . ? C00C C00B C007 119.11(16) . . ? C00I C00B C007 118.86(16) . . ? C00I C00B C00C 122.02(16) . . ? C00F C00C C00B 121.15(17) . . ? C009 C00D C00F 121.27(17) . . ? C00G C00E C008 120.79(16) . . ? C00M C00E C008 121.54(16) . . ? C00M C00E C00G 117.67(16) . . ? C00C C00F C00D 119.96(17) . . ? C00J C00G C00E 121.51(17) . . ? C00J C00H N005 118.08(17) . . ? C00L C00H N005 120.24(17) . . ? C00L C00H C00J 121.69(17) . . ? C00K C00I C00B 121.31(17) . . ? C00G C00J C00H 118.87(17) . . ? C00I C00K C008 120.72(17) . . ? C00H C00L C00M 119.01(18) . . ? C00L C00M C00E 121.24(18) . . ? _shelx_res_file ; TITL dm_skp_3_219_autored_a.res in P2(1)/c dm_skp_3_219_autored.res created by SHELXL-2018/3 at 15:43:46 on 17-Feb-2021 REM Old TITL DM_SKP_3_219_autored in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.160, Rweak 0.019, Alpha 0.027 REM 0.582 for 129 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N2 O2 CELL 0.71073 4.9733 15.3701 19.3784 90 92.471 90 ZERR 6 0.0002 0.0006 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 56 8 12 L.S. 4 PLAN 20 0 0 SIZE 0.05 0.06 0.12 TEMP -123 BOND list 4 fmap 2 ACTA REM REM REM WGHT 0.072900 0.200400 FVAR 0.57588 O001 4 0.042305 0.517665 0.366586 11.00000 0.01955 0.03983 = 0.05663 -0.00908 -0.00650 -0.00221 O002 4 0.912046 0.053107 0.555218 11.00000 0.06766 0.04633 = 0.04783 0.00452 -0.01848 0.01411 N003 3 -0.398453 0.533977 0.382889 11.00000 0.02091 0.03783 = 0.05001 -0.01178 -0.00415 -0.00086 AFIX 43 H003 2 -0.564319 0.519464 0.370053 11.00000 -1.20000 AFIX 0 O004 4 1.100030 0.180131 0.555361 11.00000 0.04911 0.06792 = 0.05496 0.00709 -0.02342 -0.00472 N005 3 0.931010 0.128176 0.533795 11.00000 0.04006 0.04793 = 0.03304 0.00254 -0.00522 0.01243 C006 1 0.059287 0.327666 0.329848 11.00000 0.02401 0.02765 = 0.02770 0.00050 -0.00419 -0.00081 AFIX 43 H006 2 0.119513 0.363908 0.367101 11.00000 -1.20000 AFIX 0 C007 1 -0.141056 0.359615 0.281971 11.00000 0.02012 0.02786 = 0.03002 0.00426 -0.00199 -0.00267 C008 1 0.168978 0.246111 0.324121 11.00000 0.02586 0.03044 = 0.02938 0.00186 -0.00396 0.00163 C009 1 -0.272921 0.441665 0.289771 11.00000 0.02017 0.02726 = 0.03323 0.00441 -0.00169 -0.00325 C00A 1 -0.194238 0.500559 0.349009 11.00000 0.02151 0.02459 = 0.04012 0.00245 -0.00463 -0.00045 C00B 1 -0.228171 0.304337 0.226176 11.00000 0.02803 0.03047 = 0.02769 0.00150 -0.00340 -0.00204 C00C 1 -0.436597 0.333341 0.179367 11.00000 0.03521 0.03564 = 0.02899 0.00130 -0.00797 -0.00284 AFIX 43 H00C 2 -0.492233 0.297405 0.141504 11.00000 -1.20000 AFIX 0 C00D 1 -0.477451 0.465827 0.243696 11.00000 0.02584 0.03115 = 0.03732 0.00509 -0.00458 0.00005 AFIX 43 H00D 2 -0.565858 0.519924 0.249678 11.00000 -1.20000 AFIX 0 C00E 1 0.367861 0.214475 0.377668 11.00000 0.02745 0.03393 = 0.03100 -0.00082 -0.00174 0.00513 C00F 1 -0.558375 0.411905 0.187806 11.00000 0.02975 0.03833 = 0.03449 0.00918 -0.00991 -0.00219 AFIX 43 H00F 2 -0.697698 0.430252 0.156008 11.00000 -1.20000 AFIX 0 C00G 1 0.533657 0.273157 0.415422 11.00000 0.02942 0.03249 = 0.03660 0.00358 -0.00133 0.00103 AFIX 43 H00G 2 0.518210 0.333676 0.406113 11.00000 -1.20000 AFIX 0 C00H 1 0.737488 0.156848 0.479187 11.00000 0.03053 0.04074 = 0.03010 0.00137 -0.00683 0.00831 C00I 1 -0.107623 0.221398 0.220146 11.00000 0.03862 0.03438 = 0.03308 -0.00403 -0.00768 0.00147 AFIX 43 H00I 2 -0.160362 0.185008 0.182315 11.00000 -1.20000 AFIX 0 C00J 1 0.717878 0.244929 0.465571 11.00000 0.02937 0.04001 = 0.03217 -0.00010 -0.00180 0.00017 AFIX 43 H00J 2 0.829622 0.285314 0.490395 11.00000 -1.20000 AFIX 0 C00K 1 0.082639 0.192712 0.267547 11.00000 0.03927 0.03195 = 0.03679 -0.00315 -0.00515 0.00637 AFIX 43 H00K 2 0.158331 0.136407 0.262703 11.00000 -1.20000 AFIX 0 C00L 1 0.580415 0.096816 0.443199 11.00000 0.04761 0.03145 = 0.03565 -0.00028 -0.00921 0.01199 AFIX 43 H00L 2 0.598489 0.036446 0.452839 11.00000 -1.20000 AFIX 0 C00M 1 0.395998 0.125817 0.392816 11.00000 0.04149 0.03271 = 0.03787 -0.00380 -0.01005 0.00522 AFIX 43 H00M 2 0.286462 0.084773 0.368050 11.00000 -1.20000 AFIX 0 C00N 1 -0.353948 0.593584 0.440304 11.00000 0.03457 0.05363 = 0.06604 -0.02820 -0.00466 0.00334 AFIX 137 H00A 2 -0.267643 0.646646 0.424040 11.00000 -1.50000 H00B 2 -0.237268 0.565948 0.475975 11.00000 -1.50000 H00E 2 -0.526872 0.608419 0.459679 11.00000 -1.50000 AFIX 0 HKLF 4 REM dm_skp_3_219_autored_a.res in P2(1)/c REM wR2 = 0.1836, GooF = S = 1.034, Restrained GooF = 1.034 for all data REM R1 = 0.0756 for 2689 Fo > 4sig(Fo) and 0.1927 for all 5498 data REM 209 parameters refined using 0 restraints END WGHT 0.0726 0.1999 REM Highest difference peak 0.316, deepest hole -0.257, 1-sigma level 0.056 Q1 1 0.9346 0.2337 0.5206 11.00000 0.05 0.32 Q2 1 -0.0645 0.3428 0.3093 11.00000 0.05 0.28 Q3 1 -0.3205 0.3187 0.1987 11.00000 0.05 0.26 Q4 1 -0.3352 0.4593 0.2600 11.00000 0.05 0.24 Q5 1 -0.1920 0.3352 0.2595 11.00000 0.05 0.23 Q6 1 0.2601 0.2308 0.3495 11.00000 0.05 0.22 Q7 1 0.0225 0.2195 0.2361 11.00000 0.05 0.22 Q8 1 1.2465 0.1208 0.5032 11.00000 0.05 0.19 Q9 1 -0.4305 0.5760 0.5020 11.00000 0.05 0.19 Q10 1 0.0380 0.4799 0.3983 11.00000 0.05 0.18 Q11 1 0.1265 0.2210 0.3083 11.00000 0.05 0.18 Q12 1 0.1832 0.0815 0.3852 11.00000 0.05 0.18 Q13 1 -0.2520 0.4631 0.3128 11.00000 0.05 0.18 Q14 1 0.0860 0.2778 0.3317 11.00000 0.05 0.18 Q15 1 1.0489 0.2787 0.5729 11.00000 0.05 0.18 Q16 1 -0.4707 0.6419 0.4181 11.00000 0.05 0.17 Q17 1 0.5928 0.2523 0.4516 11.00000 0.05 0.17 Q18 1 -0.2450 0.3932 0.2998 11.00000 0.05 0.17 Q19 1 -0.1548 0.2055 0.2203 11.00000 0.05 0.17 Q20 1 0.2170 0.1354 0.2430 11.00000 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492.54 30.53 0 5 -3 498.63 30.93 0 5 4 24.58 6.22 0 -5 4 21.75 6.17 0 5 4 10.99 4.95 0 -5 4 19.23 5.02 0 5 -4 26.93 7.03 0 -5 -4 21.68 6.73 0 5 -4 21.53 5.77 0 -5 -4 14.43 4.48 0 -5 4 22.76 6.01 0 5 -4 20.32 6.28 0 5 -4 22.30 6.17 0 -5 4 20.90 6.22 0 5 4 16.76 5.95 0 -5 -4 19.30 2.68 0 5 4 26.69 8.34 0 -5 4 36.13 8.72 0 -5 -4 16.57 6.47 0 5 4 20.85 5.27 0 5 -4 22.73 7.50 0 -5 -4 16.83 5.41 0 5 4 19.91 5.40 0 5 -4 22.99 7.43 0 -5 -4 30.00 6.85 0 5 -4 23.69 5.65 0 -5 4 20.37 6.36 0 -5 -4 23.64 6.06 0 5 4 20.12 6.22 0 5 -5 154.28 16.49 0 -5 5 141.20 16.27 0 -5 5 140.73 15.82 0 5 -5 147.46 14.28 0 5 5 139.93 17.44 0 5 -5 175.98 17.91 0 -5 5 158.33 14.63 0 -5 -5 173.13 18.43 0 5 5 152.74 16.79 0 -5 -5 159.22 16.85 0 5 -5 131.65 16.33 0 -5 5 147.13 16.91 0 -5 5 147.81 18.97 0 5 -5 169.69 14.85 0 5 5 150.40 14.51 0 -5 -5 145.78 18.01 0 -5 -5 148.98 14.87 0 5 5 160.15 19.21 0 -5 -5 154.15 15.28 0 5 -5 149.30 19.15 0 5 5 163.11 17.28 0 5 -5 141.85 17.74 0 -5 -5 132.66 15.15 0 5 5 118.26 16.64 0 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12 -3 102.95 21.95 0 12 3 82.12 20.37 0 12 3 70.88 18.13 0 12 -3 65.21 17.10 0 12 3 71.40 21.04 0 12 -3 62.51 16.24 0 12 -3 80.54 21.53 0 12 -3 87.36 19.92 0 12 3 59.77 15.41 0 -12 -3 77.70 15.60 0 12 3 75.73 20.93 0 12 -3 77.69 17.63 0 -12 -3 71.58 17.50 0 -12 3 53.45 15.41 0 12 -4 16.45 9.81 0 -12 -4 17.22 9.53 0 -12 4 29.85 12.28 0 12 -4 16.18 7.32 0 12 4 18.12 6.36 0 -12 4 24.90 9.86 0 12 -4 28.62 10.19 0 -12 4 17.46 8.76 0 -12 -4 16.47 5.10 0 12 4 28.32 12.95 0 12 4 16.07 9.86 0 12 -4 2.67 5.37 0 12 -4 17.56 9.91 0 12 -4 16.24 6.14 0 12 4 16.42 9.81 0 12 -4 35.62 15.15 0 12 4 14.61 5.88 0 12 4 23.60 10.69 0 12 -4 15.72 8.16 0 12 4 15.56 6.80 0 -12 -4 26.85 11.29 0 12 4 25.85 10.86 0 12 -4 18.95 8.81 0 -12 -5 -7.54 6.57 0 12 -5 -1.28 5.48 0 12 -5 5.44 3.94 0 -12 5 6.29 7.08 0 12 5 11.24 8.09 0 12 -5 -0.57 3.80 0 -12 -5 8.30 4.03 0 12 5 6.72 7.51 0 12 -5 9.15 6.86 0 -12 5 9.60 8.16 0 -12 5 8.70 5.64 0 12 5 11.90 8.69 0 12 -5 26.63 11.05 0 12 5 1.58 8.13 0 12 5 0.20 4.37 0 -12 -5 4.99 4.54 0 12 -5 2.15 3.28 0 12 -5 8.05 5.84 0 12 5 11.85 7.66 0 12 5 10.65 7.24 0 12 -6 443.88 45.00 0 12 -6 384.38 38.83 0 -12 6 397.89 42.66 0 12 6 300.76 40.55 0 -12 -6 432.72 46.47 0 -12 6 428.17 39.51 0 12 -6 399.53 36.33 0 -12 -6 375.97 22.53 0 12 -6 402.76 42.40 0 12 6 375.20 42.52 0 -12 6 404.10 44.73 0 12 6 380.72 40.04 0 12 -6 431.31 38.77 0 12 6 402.20 48.31 0 -12 6 350.19 43.62 0 12 -6 399.69 43.75 0 12 -6 378.37 44.52 0 12 6 406.62 43.77 0 12 -6 435.70 46.19 0 -12 6 396.02 43.59 0 -12 -6 402.14 38.36 0 12 6 362.86 43.44 0 12 6 396.63 38.27 0 -12 -6 356.00 41.34 0 12 7 40.27 11.83 0 -12 -7 36.18 13.89 0 12 -7 17.62 6.62 0 12 -7 2.97 6.66 0 -12 7 21.25 12.53 0 12 7 8.94 7.42 0 12 7 19.98 11.70 0 -12 7 24.45 13.65 0 -12 -7 20.58 4.15 0 12 -7 10.60 9.55 0 -12 7 5.72 7.34 0 12 7 14.51 7.85 0 12 7 22.47 15.28 0 12 -7 26.35 11.27 0 -12 7 17.82 12.49 0 12 -7 5.51 3.84 0 12 7 16.43 10.17 0 12 -7 12.57 9.79 0 -12 -7 1.62 5.12 0 -12 7 20.98 9.97 0 12 -7 8.04 6.67 0 -12 -7 23.30 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22.00 -7 -2 -5 -18.11 16.94 -7 -2 -6 27.34 20.94 -7 -3 12 19.64 17.22 -7 3 10 11.55 16.08 -7 -3 10 -1.05 12.74 -7 3 9 45.71 22.40 -7 -3 9 -21.99 21.34 -7 -3 8 27.83 14.04 -7 3 8 40.29 21.29 -7 -3 8 49.80 20.08 -7 3 8 22.38 14.82 -7 -3 7 20.75 17.51 -7 3 7 12.08 12.24 -7 -3 7 26.57 18.66 -7 3 7 5.73 11.17 -7 3 7 1.85 4.59 -7 -3 6 4.73 13.39 -7 3 6 2.52 16.65 -7 3 6 2.60 8.60 -7 3 6 11.72 10.28 -7 -3 6 27.73 18.78 -7 -3 5 -0.58 9.79 -7 3 5 10.30 18.44 -7 -3 5 -14.14 8.61 -7 3 5 0.16 8.11 -7 -3 5 7.61 9.91 -7 3 5 15.23 12.05 -7 -3 5 -13.12 14.23 -7 -3 4 -23.77 18.12 -7 3 4 9.89 12.98 -7 -3 4 13.18 14.36 -7 3 4 10.54 12.74 -7 -3 4 1.83 11.56 -7 3 4 2.27 15.53 -7 -3 4 9.15 14.35 -7 -3 3 6.65 14.01 -7 3 3 25.84 15.65 -7 -3 3 11.92 14.33 -7 -3 3 18.19 15.95 -7 3 3 8.31 11.75 -7 -3 3 -11.93 18.21 -7 -3 2 1.64 16.60 -7 -3 2 13.27 9.10 -7 3 2 -7.10 12.15 -7 -3 2 30.10 22.90 -7 3 2 6.18 12.47 -7 -3 1 -4.19 11.84 -7 3 1 22.76 19.08 -7 -3 1 27.23 21.27 -7 3 1 -7.40 16.69 -7 -3 1 -26.45 17.09 -7 -3 0 -28.60 23.62 -7 3 0 -45.29 24.61 -7 -3 0 -3.66 12.16 -7 3 0 20.35 15.16 -7 -3 0 -20.06 20.88 -7 -3 -1 -28.14 24.75 -7 3 -1 17.81 16.79 -7 -3 -1 -5.11 9.52 -7 3 -1 1.28 14.59 -7 3 -1 -10.77 18.80 -7 -3 -1 -10.85 18.08 -7 -3 -2 -32.19 28.14 -7 3 -2 13.17 19.34 -7 -3 -2 -9.87 10.33 -7 3 -2 -11.18 22.58 -7 -3 -2 -14.06 14.03 -7 -3 -3 24.67 19.05 -7 3 -3 47.17 26.78 -7 3 -3 5.61 16.98 -7 -3 -5 -15.03 11.85 -7 -3 -6 -8.12 15.52 -7 4 11 -6.87 17.87 -7 4 10 -19.05 20.91 -7 -4 10 -5.78 14.48 -7 4 9 15.11 14.68 -7 -4 9 -8.75 17.51 -7 4 8 1.74 10.66 -7 -4 8 0.87 17.89 -7 -4 7 -0.79 13.76 -7 -4 7 -7.39 9.90 -7 4 7 -16.31 13.78 -7 4 7 -10.65 6.15 -7 -4 6 5.56 12.97 -7 -4 6 9.34 12.44 -7 4 6 9.04 7.79 -7 4 6 21.59 15.51 -7 -4 5 1.76 17.63 -7 -4 5 -1.54 10.98 -7 4 5 27.37 13.58 -7 -4 5 -5.10 17.93 -7 4 5 -30.06 22.19 -7 -4 4 46.17 26.14 -7 -4 4 -7.46 11.28 -7 4 4 -7.93 14.77 -7 -4 4 0.55 11.43 -7 4 4 9.81 17.90 -7 -4 3 5.41 16.80 -7 4 3 16.33 16.89 -7 -4 3 -11.19 14.94 -7 -4 3 9.25 13.50 -7 4 3 41.25 22.99 -7 -4 2 -16.84 21.12 -7 4 2 24.93 19.71 -7 -4 2 -16.98 14.59 -7 4 2 -12.38 12.03 -7 -4 2 35.44 24.77 -7 4 2 34.54 19.11 -7 -4 2 -12.18 17.20 -7 4 1 4.21 11.47 -7 -4 1 -6.45 14.42 -7 4 1 14.49 14.06 -7 4 1 4.58 14.38 -7 -4 1 10.79 12.31 -7 -4 0 -1.06 19.56 -7 4 0 -15.53 17.83 -7 -4 0 3.05 8.68 -7 4 0 1.48 10.28 -7 -4 0 4.87 10.73 -7 -4 -1 -0.73 17.20 -7 4 -1 -0.34 16.84 -7 -4 -1 28.68 15.06 -7 4 -1 49.07 28.96 -7 4 -1 14.49 16.40 -7 -4 -1 -16.45 20.33 -7 -4 -2 -2.28 21.33 -7 4 -2 -5.50 12.28 -7 -4 -2 22.52 17.26 -7 -4 -3 2.71 13.38 -7 4 -3 53.61 30.01 -7 -4 -5 27.70 21.95 -7 -4 -6 23.92 21.45 -7 5 11 -6.84 12.35 -7 5 10 -14.48 17.88 -7 5 9 -27.53 23.06 -7 5 8 -31.30 20.75 -7 -5 7 12.85 19.35 -7 5 7 -9.73 15.73 -7 5 7 22.92 19.62 -7 5 7 -5.99 4.87 -7 -5 6 -27.97 19.00 -7 5 6 5.73 12.60 -7 5 6 0.56 7.02 -7 5 6 8.05 15.31 -7 -5 5 31.77 23.29 -7 5 5 -0.64 14.67 -7 -5 5 11.78 16.95 -7 5 5 1.16 7.14 -7 -5 5 -26.21 21.75 -7 5 5 20.56 15.45 -7 -5 4 -9.53 14.51 -7 5 4 31.26 19.71 -7 -5 4 4.54 12.25 -7 5 4 9.89 7.99 -7 5 4 0.59 11.30 -7 -5 3 -7.06 17.74 -7 5 3 -10.24 11.22 -7 -5 3 33.39 21.48 -7 5 3 -4.93 15.35 -7 5 2 8.38 14.15 -7 -5 2 -0.34 14.61 -7 5 2 -7.81 15.25 -7 5 2 -10.28 13.38 -7 -5 1 -23.33 17.18 -7 -5 1 23.48 22.62 -7 5 1 8.85 16.12 -7 5 1 11.30 14.34 -7 -5 1 18.73 20.74 -7 -5 0 11.96 14.62 -7 -5 0 32.18 22.95 -7 5 0 36.69 22.58 -7 5 0 28.32 21.97 -7 5 0 -29.23 17.93 -7 -5 0 19.53 15.85 -7 -5 -1 27.96 21.17 -7 -5 -1 -5.55 13.45 -7 5 -1 -29.64 21.49 -7 -5 -2 30.23 20.61 -7 -5 -2 -4.21 21.81 -7 5 -2 27.75 20.29 -7 -5 -3 11.91 15.30 -7 6 11 -1.28 14.19 -7 -6 11 -24.73 21.85 -7 6 10 20.03 17.91 -7 -6 10 -29.74 23.97 -7 6 9 33.32 23.09 -7 -6 9 22.21 19.83 -7 6 8 16.48 23.18 -7 -6 8 -10.35 17.33 -7 6 7 4.33 16.65 -7 -6 7 7.33 13.44 -7 6 7 5.35 3.41 -7 -6 6 40.56 21.94 -7 6 6 -3.70 19.20 -7 -6 6 -21.37 17.57 -7 6 6 -8.79 6.94 -7 6 6 -1.93 14.84 -7 -6 5 13.34 15.45 -7 6 5 25.19 20.66 -7 -6 5 3.95 11.38 -7 6 5 1.82 9.52 -7 6 5 26.88 17.96 -7 -6 4 -26.13 15.49 -7 6 4 -3.44 11.66 -7 -6 4 -13.43 14.34 -7 6 4 13.62 17.84 -7 6 3 -9.06 17.41 -7 -6 3 -2.05 12.78 -7 6 3 9.08 9.78 -7 6 3 29.41 18.17 -7 -6 2 -18.11 20.86 -7 6 2 -6.73 8.75 -7 -6 1 9.06 17.57 -7 6 1 41.21 24.74 -7 -6 0 -3.62 15.40 -7 6 0 16.06 17.74 -7 -6 -1 -32.18 21.87 -7 6 -1 45.20 26.04 -7 6 -2 37.64 26.89 -7 -7 11 17.92 15.45 -7 -7 10 -33.53 23.19 -7 -7 9 -21.04 19.92 -7 -7 8 38.34 22.45 -7 -7 7 0.33 14.94 -7 -7 6 -12.57 17.06 -7 -7 6 17.16 18.56 -7 7 6 8.51 11.98 -7 -7 5 21.98 21.72 -7 7 5 -25.23 13.21 -7 7 5 -5.95 14.69 -7 -7 4 13.22 13.51 -7 7 4 -7.79 12.40 -7 7 3 -7.34 10.03 -7 -7 2 -26.28 23.18 -7 7 2 -10.76 13.91 -7 -7 1 26.87 19.57 -7 7 1 0.35 14.06 -7 -7 0 42.81 25.36 -7 7 0 -1.10 16.11 -7 7 -1 -41.84 28.42 -7 -8 5 -10.73 16.17 -7 8 5 3.73 10.42 -7 8 5 33.81 27.80 -7 8 4 18.38 11.65 -7 -8 3 7.01 16.04 -7 8 3 16.24 17.43 -7 8 3 19.12 24.87 -7 -8 2 5.54 16.56 -7 8 2 17.12 24.87 -7 -8 1 -28.32 22.12 -7 8 1 -15.62 21.98 -7 8 0 -10.94 17.37 -7 9 4 35.97 18.67 -7 9 4 8.64 17.78 -7 -9 3 4.77 21.33 -7 9 3 8.66 15.35 -7 9 2 60.58 29.54 -7 -10 4 0.34 15.56 -7 10 4 0.69 17.40 0 0 0 0.00 0.00 TITL DM_SKP_3_219_autored in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 4.973298 15.370110 19.378357 90.0000 92.4708 90.0000 ZERR 6.00 0.000213 0.000631 0.000864 0.0000 0.0035 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 REM CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0 TEMP -123 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 46514 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.374 _oxdiff_exptl_absorpt_empirical_full_min 0.750