data_dm_skp3_37 _audit_creation_date 2022-01-08 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _shelx_SHELXL_version_number '2014/7' _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 '0.444(C23 H23 F2 N O)' _chemical_formula_sum 'C10.22 H10.22 F0.89 N0.44 O0.44' _chemical_formula_weight 163.30 _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' 'F' 'F' 0.0171 0.0103 '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 17.568(2) _cell_length_b 7.5840(6) _cell_length_c 16.119(2) _cell_angle_alpha 90 _cell_angle_beta 112.022(14) _cell_angle_gamma 90 _cell_volume 1991.0(4) _cell_formula_units_Z 9 _cell_measurement_reflns_used 2540 _cell_measurement_temperature 150 _cell_measurement_theta_max 21.5720 _cell_measurement_theta_min 2.4720 _shelx_estimated_absorpt_T_max 0.993 _shelx_estimated_absorpt_T_min 0.983 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.05145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) 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 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.096 _exptl_crystal_size_min 0.084 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.2475 _diffrn_reflns_av_unetI/netI 0.2509 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.881 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 41848 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.881 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.707 _diffrn_reflns_theta_min 2.501 _diffrn_ambient_temperature 150 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.881 _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 -102.01 129.49 0.50 4.00 9.41 -12.98 -31.50 -- 463 2 \w -108.63 15.87 0.50 4.00 -- -12.98 -59.25 -33.92 249 3 \w -108.63 15.87 0.50 4.00 -- -12.98 -59.25 -84.92 249 4 \w -108.63 15.87 0.50 4.00 -- -12.98 -59.25-135.92 249 5 \w 13.87 15.87 0.50 4.00 -- -12.98 -59.25 20.08 4 ; _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 0.0047504000 _diffrn_orient_matrix_UB_12 0.0739644000 _diffrn_orient_matrix_UB_13 0.0284138000 _diffrn_orient_matrix_UB_21 -0.0427091000 _diffrn_orient_matrix_UB_22 -0.0012662000 _diffrn_orient_matrix_UB_23 -0.0088456000 _diffrn_orient_matrix_UB_31 0.0072473000 _diffrn_orient_matrix_UB_32 -0.0573028000 _diffrn_orient_matrix_UB_33 0.0369766000 _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 2172 _reflns_number_total 6997 _reflns_odcompleteness_completeness 87.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 33.63 _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 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.310 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 6997 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2959 _refine_ls_R_factor_gt 0.0968 _refine_ls_restrained_S_all 0.950 _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^)+(0.1320P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2313 _refine_ls_wR_factor_ref 0.3276 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00D(H00D), C00I(H00I) 2.b Aromatic/amide H refined with riding coordinates: C00B(H00B), C00C(H00C), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00M(H00M) 2.c Idealised Me refined as rotating group: C00N(H00A,H00J,H00N), C00P(H00O,H00P,H00Q), C00Q(H00R,H00S,H00T), C00R(H00U, H00V,H00W) ; _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 0.83531(14) 0.4414(3) 0.94465(15) 0.0570(7) Uani 1 1 d . . . . . F002 F 0.58179(13) -0.2370(2) 0.46056(17) 0.0843(9) Uani 1 1 d . . . . . F003 F 0.49247(15) 0.2970(3) 0.30492(15) 0.0933(9) Uani 1 1 d . . . . . N004 N 0.81049(14) 0.7297(3) 0.89856(16) 0.0418(7) Uani 1 1 d . . . . . C005 C 0.76269(18) 0.3368(4) 0.6528(2) 0.0420(8) Uani 1 1 d . . . . . C006 C 0.62728(17) 0.2190(4) 0.5344(2) 0.0439(8) Uani 1 1 d . . . . . C007 C 0.80549(18) 0.4202(4) 0.7383(2) 0.0418(8) Uani 1 1 d . . . . . C008 C 0.67449(18) 0.3183(4) 0.6221(2) 0.0434(8) Uani 1 1 d . . . . . C009 C 0.80468(18) 0.5525(4) 0.8843(2) 0.0424(8) Uani 1 1 d . . . . . C00A C 0.75943(18) 0.4855(4) 0.7893(2) 0.0427(8) Uani 1 1 d . . . . . C00B C 0.80936(19) 0.2719(4) 0.6038(2) 0.0454(8) Uani 1 1 d . . . . . H00B H 0.7819 0.2155 0.5479 0.055 Uiso 1 1 calc R U . . . C00C C 0.89338(19) 0.4355(4) 0.7696(2) 0.0475(9) Uani 1 1 d . . . . . H00C H 0.9224 0.4907 0.8255 0.057 Uiso 1 1 calc R U . . . C00D C 0.85373(19) 0.8004(4) 0.9918(2) 0.0475(9) Uani 1 1 d . . . . . H00D H 0.8501 0.9318 0.9868 0.057 Uiso 1 1 calc R U . . . C00E C 0.6751(2) 0.4711(4) 0.7556(2) 0.0498(9) Uani 1 1 d . . . . . H00E H 0.6449 0.5174 0.7888 0.060 Uiso 1 1 calc R U . . . C00F C 0.9360(2) 0.3721(5) 0.7203(2) 0.0544(9) Uani 1 1 d . . . . . H00F H 0.9941 0.3832 0.7424 0.065 Uiso 1 1 calc R U . . . C00G C 0.8936(2) 0.2890(4) 0.6356(2) 0.0510(9) Uani 1 1 d . . . . . H00G H 0.9235 0.2458 0.6014 0.061 Uiso 1 1 calc R U . . . C00H C 0.63259(19) 0.3876(4) 0.6718(2) 0.0538(10) Uani 1 1 d . . . . . H00H H 0.5744 0.3795 0.6497 0.065 Uiso 1 1 calc R U . . . C00I C 0.7801(2) 0.8604(4) 0.8244(2) 0.0507(9) Uani 1 1 d . . . . . H00I H 0.7558 0.7919 0.7675 0.061 Uiso 1 1 calc R U . . . C00J C 0.58131(19) -0.0554(4) 0.4588(3) 0.0540(10) Uani 1 1 d . . . . . C00K C 0.5818(2) 0.3071(4) 0.4584(2) 0.0564(10) Uani 1 1 d . . . . . H00K H 0.5811 0.4324 0.4569 0.068 Uiso 1 1 calc R U . . . C00L C 0.62775(19) 0.0338(4) 0.5366(2) 0.0511(9) Uani 1 1 d . . . . . H00L H 0.6588 -0.0285 0.5897 0.061 Uiso 1 1 calc R U . . . C00M C 0.5346(2) 0.0283(5) 0.3808(2) 0.0569(10) Uani 1 1 d . . . . . H00M H 0.5028 -0.0355 0.3285 0.068 Uiso 1 1 calc R U . . . C00N C 0.8106(2) 0.7475(5) 1.0553(2) 0.0601(10) Uani 1 1 d . . . . . H00A H 0.7531 0.7852 1.0298 0.090 Uiso 1 1 calc R U . . . H00J H 0.8381 0.8044 1.1135 0.090 Uiso 1 1 calc R U . . . H00N H 0.8131 0.6192 1.0630 0.090 Uiso 1 1 calc R U . . . C00O C 0.5362(2) 0.2095(5) 0.3826(2) 0.0601(10) Uani 1 1 d . . . . . C00P C 0.7114(2) 0.9753(5) 0.8323(3) 0.0671(12) Uani 1 1 d . . . . . H00O H 0.6672 0.8997 0.8352 0.101 Uiso 1 1 calc R U . . . H00P H 0.6897 1.0528 0.7800 0.101 Uiso 1 1 calc R U . . . H00Q H 0.7332 1.0470 0.8867 0.101 Uiso 1 1 calc R U . . . C00Q C 0.9460(2) 0.7547(5) 1.0289(3) 0.0664(12) Uani 1 1 d . . . . . H00R H 0.9529 0.6270 1.0378 0.100 Uiso 1 1 calc R U . . . H00S H 0.9734 0.8150 1.0862 0.100 Uiso 1 1 calc R U . . . H00T H 0.9704 0.7931 0.9863 0.100 Uiso 1 1 calc R U . . . C00R C 0.8509(2) 0.9700(5) 0.8174(3) 0.0708(12) Uani 1 1 d . . . . . H00U H 0.8704 1.0535 0.8673 0.106 Uiso 1 1 calc R U . . . H00V H 0.8314 1.0350 0.7607 0.106 Uiso 1 1 calc R U . . . H00W H 0.8959 0.8915 0.8195 0.106 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 O001 0.0802(16) 0.0387(12) 0.0439(15) 0.0058(10) 0.0138(12) 0.0036(10) F002 0.0887(16) 0.0411(11) 0.099(2) -0.0172(11) 0.0077(14) -0.0092(9) F003 0.1113(19) 0.0859(16) 0.0484(15) 0.0034(12) -0.0093(13) 0.0141(13) N004 0.0481(14) 0.0337(13) 0.0311(14) 0.0006(10) 0.0005(11) -0.0010(10) C005 0.0471(18) 0.0312(14) 0.0400(18) 0.0006(12) 0.0075(14) 0.0020(12) C006 0.0384(16) 0.0323(15) 0.052(2) -0.0065(13) 0.0062(14) -0.0015(12) C007 0.0477(18) 0.0315(14) 0.0402(19) 0.0041(12) 0.0097(15) 0.0017(12) C008 0.0465(18) 0.0334(14) 0.0406(19) -0.0022(13) 0.0053(15) -0.0002(12) C009 0.0483(18) 0.0383(16) 0.0392(19) 0.0013(13) 0.0147(15) -0.0011(13) C00A 0.0445(18) 0.0337(15) 0.0400(19) 0.0010(13) 0.0044(15) -0.0007(12) C00B 0.055(2) 0.0358(15) 0.0392(19) 0.0008(13) 0.0101(15) 0.0020(13) C00C 0.0498(19) 0.0432(17) 0.0402(19) 0.0005(13) 0.0060(16) 0.0011(13) C00D 0.0538(19) 0.0412(16) 0.0347(18) -0.0008(13) 0.0021(15) 0.0004(13) C00E 0.051(2) 0.0482(18) 0.047(2) -0.0077(15) 0.0155(16) -0.0033(14) C00F 0.0442(18) 0.060(2) 0.049(2) 0.0013(17) 0.0070(16) 0.0009(15) C00G 0.053(2) 0.0493(19) 0.048(2) 0.0017(15) 0.0164(17) 0.0057(14) C00H 0.0442(18) 0.0492(19) 0.059(2) -0.0075(17) 0.0089(17) -0.0040(14) C00I 0.063(2) 0.0360(16) 0.0363(18) 0.0012(13) -0.0004(16) 0.0027(14) C00J 0.0482(19) 0.0386(17) 0.066(3) -0.0107(15) 0.0113(18) -0.0049(13) C00K 0.070(2) 0.0411(17) 0.051(2) -0.0070(15) 0.0142(19) -0.0047(15) C00L 0.0499(18) 0.0437(17) 0.048(2) -0.0008(15) 0.0050(16) -0.0011(14) C00M 0.050(2) 0.060(2) 0.049(2) -0.0148(17) 0.0058(17) -0.0064(15) C00N 0.078(2) 0.0509(19) 0.048(2) -0.0102(16) 0.0188(19) -0.0060(16) C00O 0.064(2) 0.062(2) 0.038(2) -0.0016(16) 0.0017(17) 0.0053(16) C00P 0.063(2) 0.055(2) 0.068(3) 0.0062(18) 0.007(2) 0.0141(16) C00Q 0.060(2) 0.074(2) 0.045(2) -0.0032(18) -0.0027(18) -0.0046(17) C00R 0.076(3) 0.057(2) 0.075(3) 0.019(2) 0.024(2) -0.0065(18) _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 C009 1.246(3) . ? F002 C00J 1.378(4) . ? F003 C00O 1.370(4) . ? N004 C009 1.360(4) . ? N004 C00D 1.506(4) . ? N004 C00I 1.489(4) . ? C005 C007 1.446(4) . ? C005 C008 1.446(4) . ? C005 C00B 1.422(5) . ? C006 C008 1.541(4) . ? C006 C00K 1.362(4) . ? C006 C00L 1.405(4) . ? C007 C00A 1.440(5) . ? C007 C00C 1.438(4) . ? C008 C00H 1.379(5) . ? C009 C00A 1.525(4) . ? C00A C00E 1.378(4) . ? C00B H00B 0.9500 . ? C00B C00G 1.379(4) . ? C00C H00C 0.9500 . ? C00C C00F 1.367(5) . ? C00D H00D 1.0000 . ? C00D C00N 1.538(5) . ? C00D C00Q 1.542(5) . ? C00E H00E 0.9500 . ? C00E C00H 1.424(5) . ? C00F H00F 0.9500 . ? C00F C00G 1.433(5) . ? C00G H00G 0.9500 . ? C00H H00H 0.9500 . ? C00I H00I 1.0000 . ? C00I C00P 1.533(5) . ? C00I C00R 1.535(5) . ? C00J C00L 1.389(4) . ? C00J C00M 1.372(5) . ? C00K H00K 0.9500 . ? C00K C00O 1.396(4) . ? C00L H00L 0.9500 . ? C00M H00M 0.9500 . ? C00M C00O 1.375(5) . ? C00N H00A 0.9800 . ? C00N H00J 0.9800 . ? C00N H00N 0.9800 . ? C00P H00O 0.9800 . ? C00P H00P 0.9800 . ? C00P H00Q 0.9800 . ? C00Q H00R 0.9800 . ? C00Q H00S 0.9800 . ? C00Q H00T 0.9800 . ? C00R H00U 0.9800 . ? C00R H00V 0.9800 . ? C00R H00W 0.9800 . ? 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 C009 N004 C00D 119.9(2) . . ? C009 N004 C00I 122.7(2) . . ? C00I N004 C00D 117.3(2) . . ? C007 C005 C008 118.4(3) . . ? C00B C005 C007 118.6(3) . . ? C00B C005 C008 122.9(3) . . ? C00K C006 C008 121.3(3) . . ? C00K C006 C00L 120.6(3) . . ? C00L C006 C008 118.0(3) . . ? C00A C007 C005 119.5(3) . . ? C00C C007 C005 118.4(3) . . ? C00C C007 C00A 122.1(3) . . ? C005 C008 C006 120.0(3) . . ? C00H C008 C005 120.1(3) . . ? C00H C008 C006 119.9(3) . . ? O001 C009 N004 123.6(3) . . ? O001 C009 C00A 118.0(3) . . ? N004 C009 C00A 118.4(3) . . ? C007 C00A C009 119.7(3) . . ? C00E C00A C007 119.9(3) . . ? C00E C00A C009 120.1(3) . . ? C005 C00B H00B 119.2 . . ? C00G C00B C005 121.5(3) . . ? C00G C00B H00B 119.2 . . ? C007 C00C H00C 119.4 . . ? C00F C00C C007 121.3(3) . . ? C00F C00C H00C 119.4 . . ? N004 C00D H00D 106.3 . . ? N004 C00D C00N 112.4(3) . . ? N004 C00D C00Q 111.7(3) . . ? C00N C00D H00D 106.3 . . ? C00N C00D C00Q 113.1(3) . . ? C00Q C00D H00D 106.3 . . ? C00A C00E H00E 119.6 . . ? C00A C00E C00H 120.9(3) . . ? C00H C00E H00E 119.6 . . ? C00C C00F H00F 119.8 . . ? C00C C00F C00G 120.4(3) . . ? C00G C00F H00F 119.8 . . ? C00B C00G C00F 119.8(3) . . ? C00B C00G H00G 120.1 . . ? C00F C00G H00G 120.1 . . ? C008 C00H C00E 121.1(3) . . ? C008 C00H H00H 119.5 . . ? C00E C00H H00H 119.5 . . ? N004 C00I H00I 107.0 . . ? N004 C00I C00P 111.6(3) . . ? N004 C00I C00R 111.3(2) . . ? C00P C00I H00I 107.0 . . ? C00P C00I C00R 112.5(3) . . ? C00R C00I H00I 107.0 . . ? F002 C00J C00L 118.1(3) . . ? C00M C00J F002 118.6(3) . . ? C00M C00J C00L 123.3(3) . . ? C006 C00K H00K 120.7 . . ? C006 C00K C00O 118.6(3) . . ? C00O C00K H00K 120.7 . . ? C006 C00L H00L 121.0 . . ? C00J C00L C006 117.9(3) . . ? C00J C00L H00L 121.0 . . ? C00J C00M H00M 121.9 . . ? C00J C00M C00O 116.2(3) . . ? C00O C00M H00M 121.9 . . ? C00D C00N H00A 109.5 . . ? C00D C00N H00J 109.5 . . ? C00D C00N H00N 109.5 . . ? H00A C00N H00J 109.5 . . ? H00A C00N H00N 109.5 . . ? H00J C00N H00N 109.5 . . ? F003 C00O C00K 118.9(3) . . ? F003 C00O C00M 117.7(3) . . ? C00M C00O C00K 123.3(3) . . ? C00I C00P H00O 109.5 . . ? C00I C00P H00P 109.5 . . ? C00I C00P H00Q 109.5 . . ? H00O C00P H00P 109.5 . . ? H00O C00P H00Q 109.5 . . ? H00P C00P H00Q 109.5 . . ? C00D C00Q H00R 109.5 . . ? C00D C00Q H00S 109.5 . . ? C00D C00Q H00T 109.5 . . ? H00R C00Q H00S 109.5 . . ? H00R C00Q H00T 109.5 . . ? H00S C00Q H00T 109.5 . . ? C00I C00R H00U 109.5 . . ? C00I C00R H00V 109.5 . . ? C00I C00R H00W 109.5 . . ? H00U C00R H00V 109.5 . . ? H00U C00R H00W 109.5 . . ? H00V C00R H00W 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 O001 C009 C00A C007 -75.6(4) . . . . ? O001 C009 C00A C00E 97.9(4) . . . . ? F002 C00J C00L C006 179.8(3) . . . . ? F002 C00J C00M C00O 180.0(3) . . . . ? N004 C009 C00A C007 103.4(3) . . . . ? N004 C009 C00A C00E -83.1(4) . . . . ? C005 C007 C00A C009 172.4(2) . . . . ? C005 C007 C00A C00E -1.2(4) . . . . ? C005 C007 C00C C00F -0.4(4) . . . . ? C005 C008 C00H C00E -2.9(5) . . . . ? C005 C00B C00G C00F 0.7(4) . . . . ? C006 C008 C00H C00E 176.4(3) . . . . ? C006 C00K C00O F003 -177.9(4) . . . . ? C006 C00K C00O C00M 0.3(6) . . . . ? C007 C005 C008 C006 -175.8(3) . . . . ? C007 C005 C008 C00H 3.4(4) . . . . ? C007 C005 C00B C00G -0.9(4) . . . . ? C007 C00A C00E C00H 1.8(4) . . . . ? C007 C00C C00F C00G 0.2(5) . . . . ? C008 C005 C007 C00A -1.4(4) . . . . ? C008 C005 C007 C00C 178.8(3) . . . . ? C008 C005 C00B C00G -178.9(3) . . . . ? C008 C006 C00K C00O -176.0(3) . . . . ? C008 C006 C00L C00J 176.4(3) . . . . ? C009 N004 C00D C00N -63.3(4) . . . . ? C009 N004 C00D C00Q 65.1(4) . . . . ? C009 N004 C00I C00P 117.8(3) . . . . ? C009 N004 C00I C00R -115.5(3) . . . . ? C009 C00A C00E C00H -171.7(3) . . . . ? C00A C007 C00C C00F 179.8(3) . . . . ? C00A C00E C00H C008 0.2(5) . . . . ? C00B C005 C007 C00A -179.5(3) . . . . ? C00B C005 C007 C00C 0.7(4) . . . . ? C00B C005 C008 C006 2.2(4) . . . . ? C00B C005 C008 C00H -178.6(3) . . . . ? C00C C007 C00A C009 -7.8(4) . . . . ? C00C C007 C00A C00E 178.6(3) . . . . ? C00C C00F C00G C00B -0.4(5) . . . . ? C00D N004 C009 O001 -1.8(5) . . . . ? C00D N004 C009 C00A 179.2(3) . . . . ? C00D N004 C00I C00P -66.0(3) . . . . ? C00D N004 C00I C00R 60.7(4) . . . . ? C00I N004 C009 O001 174.3(3) . . . . ? C00I N004 C009 C00A -4.7(4) . . . . ? C00I N004 C00D C00N 120.3(3) . . . . ? C00I N004 C00D C00Q -111.2(3) . . . . ? C00J C00M C00O F003 177.8(3) . . . . ? C00J C00M C00O C00K -0.4(6) . . . . ? C00K C006 C008 C005 -105.0(4) . . . . ? C00K C006 C008 C00H 75.7(4) . . . . ? C00K C006 C00L C00J 0.7(5) . . . . ? C00L C006 C008 C005 79.3(4) . . . . ? C00L C006 C008 C00H -99.9(4) . . . . ? C00L C006 C00K C00O -0.5(5) . . . . ? C00L C00J C00M C00O 0.7(6) . . . . ? C00M C00J C00L C006 -0.9(6) . . . . ? _shelx_res_file ; dm_skp3_37.res created by SHELXL-2014/7 TITL dm_skp3_37_a.res in P2(1)/c REM Old TITL dm_skp3_37_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.261, Rweak 0.025, Alpha 0.045 REM 0.457 for 323 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N O3 CELL 0.71073 17.5679 7.584 16.1194 90 112.022 90 ZERR 9 0.0023 0.0006 0.0021 0 0.014 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O UNIT 92 92 8 4 4 L.S. 10 PLAN 2 SIZE 0.084 0.096 0.2 TEMP -123.15 CONF list 4 MORE -1 BOND $H fmap 2 acta OMIT -5 9 1 REM REM REM WGHT 0.132000 FVAR 0.51460 O001 5 0.835310 0.441431 0.944648 11.00000 0.08019 0.03866 = 0.04386 0.00583 0.01384 0.00362 F002 3 0.581790 -0.236979 0.460564 11.00000 0.08867 0.04114 = 0.09917 -0.01717 0.00771 -0.00918 F003 3 0.492473 0.297031 0.304922 11.00000 0.11133 0.08589 = 0.04836 0.00343 -0.00926 0.01414 N004 4 0.810486 0.729651 0.898561 11.00000 0.04810 0.03365 = 0.03108 0.00062 0.00055 -0.00098 C005 1 0.762692 0.336843 0.652757 11.00000 0.04707 0.03123 = 0.03995 0.00061 0.00750 0.00204 C006 1 0.627280 0.219032 0.534439 11.00000 0.03842 0.03228 = 0.05157 -0.00650 0.00622 -0.00150 C007 1 0.805492 0.420239 0.738341 11.00000 0.04771 0.03150 = 0.04015 0.00406 0.00969 0.00169 C008 1 0.674489 0.318293 0.622122 11.00000 0.04654 0.03340 = 0.04059 -0.00218 0.00531 -0.00018 C009 1 0.804684 0.552495 0.884349 11.00000 0.04828 0.03829 = 0.03924 0.00127 0.01466 -0.00114 C00A 1 0.759435 0.485514 0.789293 11.00000 0.04451 0.03371 = 0.03995 0.00101 0.00444 -0.00073 C00B 1 0.809364 0.271922 0.603796 11.00000 0.05482 0.03575 = 0.03917 0.00079 0.01006 0.00202 AFIX 43 H00B 2 0.781853 0.215471 0.547884 11.00000 -1.20000 AFIX 0 C00C 1 0.893382 0.435490 0.769566 11.00000 0.04975 0.04324 = 0.04016 0.00052 0.00604 0.00111 AFIX 43 H00C 2 0.922357 0.490656 0.825483 11.00000 -1.20000 AFIX 0 C00D 1 0.853729 0.800379 0.991805 11.00000 0.05384 0.04123 = 0.03468 -0.00081 0.00210 0.00041 AFIX 13 H00D 2 0.850087 0.931790 0.986787 11.00000 -1.20000 AFIX 0 C00E 1 0.675122 0.471062 0.755629 11.00000 0.05137 0.04818 = 0.04727 -0.00774 0.01546 -0.00327 AFIX 43 H00E 2 0.644948 0.517409 0.788780 11.00000 -1.20000 AFIX 0 C00F 1 0.936028 0.372113 0.720313 11.00000 0.04417 0.06039 = 0.04935 0.00130 0.00705 0.00092 AFIX 43 H00F 2 0.994106 0.383218 0.742366 11.00000 -1.20000 AFIX 0 C00G 1 0.893626 0.289013 0.635599 11.00000 0.05341 0.04928 = 0.04809 0.00172 0.01639 0.00567 AFIX 43 H00G 2 0.923490 0.245810 0.601438 11.00000 -1.20000 AFIX 0 C00H 1 0.632586 0.387574 0.671797 11.00000 0.04421 0.04921 = 0.05876 -0.00749 0.00890 -0.00400 AFIX 43 H00H 2 0.574401 0.379484 0.649743 11.00000 -1.20000 AFIX 0 C00I 1 0.780090 0.860373 0.824417 11.00000 0.06321 0.03601 = 0.03632 0.00124 -0.00040 0.00268 AFIX 13 H00I 2 0.755765 0.791948 0.767485 11.00000 -1.20000 AFIX 0 C00J 1 0.581314 -0.055359 0.458769 11.00000 0.04819 0.03862 = 0.06635 -0.01065 0.01134 -0.00493 C00K 1 0.581793 0.307128 0.458360 11.00000 0.07028 0.04112 = 0.05059 -0.00703 0.01424 -0.00470 AFIX 43 H00K 2 0.581076 0.432357 0.456889 11.00000 -1.20000 AFIX 0 C00L 1 0.627749 0.033826 0.536629 11.00000 0.04985 0.04368 = 0.04811 -0.00079 0.00502 -0.00115 AFIX 43 H00L 2 0.658839 -0.028463 0.589679 11.00000 -1.20000 AFIX 0 C00M 1 0.534557 0.028256 0.380804 11.00000 0.05031 0.05998 = 0.04923 -0.01478 0.00585 -0.00643 AFIX 43 H00M 2 0.502800 -0.035481 0.328525 11.00000 -1.20000 AFIX 0 C00N 1 0.810569 0.747491 1.055281 11.00000 0.07776 0.05086 = 0.04751 -0.01022 0.01884 -0.00600 AFIX 137 H00A 2 0.753051 0.785227 1.029815 11.00000 -1.50000 H00J 2 0.838077 0.804375 1.113507 11.00000 -1.50000 H00N 2 0.813073 0.619165 1.062977 11.00000 -1.50000 AFIX 0 C00O 1 0.536246 0.209466 0.382593 11.00000 0.06437 0.06220 = 0.03849 -0.00163 0.00173 0.00526 C00P 1 0.711354 0.975329 0.832285 11.00000 0.06311 0.05502 = 0.06757 0.00618 0.00666 0.01409 AFIX 137 H00O 2 0.667194 0.899685 0.835188 11.00000 -1.50000 H00P 2 0.689709 1.052794 0.779970 11.00000 -1.50000 H00Q 2 0.733210 1.047009 0.886727 11.00000 -1.50000 AFIX 0 C00Q 1 0.946016 0.754708 1.028900 11.00000 0.06026 0.07401 = 0.04534 -0.00322 -0.00275 -0.00456 AFIX 137 H00R 2 0.952934 0.626988 1.037765 11.00000 -1.50000 H00S 2 0.973371 0.814971 1.086214 11.00000 -1.50000 H00T 2 0.970380 0.793146 0.986291 11.00000 -1.50000 AFIX 0 C00R 1 0.850855 0.969986 0.817351 11.00000 0.07642 0.05739 = 0.07474 0.01949 0.02375 -0.00655 AFIX 137 H00U 2 0.870441 1.053459 0.867334 11.00000 -1.50000 H00V 2 0.831443 1.035031 0.760684 11.00000 -1.50000 H00W 2 0.895864 0.891457 0.819523 11.00000 -1.50000 AFIX 0 HKLF 4 REM dm_skp3_37_a.res in P2(1)/c REM R1 = 0.0968 for 2172 Fo > 4sig(Fo) and 0.2959 for all 6997 data REM 248 parameters refined using 0 restraints END WGHT 0.1332 0.0000 REM Highest difference peak 0.310, deepest hole -0.342, 1-sigma level 0.065 Q1 1 0.6401 0.2533 0.4929 11.00000 0.05 0.31 Q2 1 0.6469 0.6670 0.6922 11.00000 0.05 0.21 ; _shelx_res_checksum 33767 _shelx_hkl_file ; -2 0 0 1298.49 40.29 2 0 0 1264.79 38.38 2 0 0 1171.54 23.85 -2 0 0 1190.98 30.41 2 0 0 1287.30 32.88 -2 0 0 1264.63 24.67 -2 0 0 1365.46 25.45 2 0 0 1142.19 23.25 -3 0 0 4533.47 90.62 3 0 0 4540.45 87.75 3 0 0 4436.01 76.13 -3 0 0 3586.54 64.81 -3 0 0 3580.56 51.67 3 0 0 4479.53 57.58 -3 0 0 4492.86 58.58 3 0 0 3945.04 52.61 -4 0 0 792.95 44.81 4 0 0 643.31 38.36 -4 0 0 531.48 23.06 4 0 0 707.96 35.01 -4 0 0 552.98 29.32 4 0 0 657.85 25.73 4 0 0 553.58 22.79 -4 0 0 523.01 23.00 -5 0 0 1523.51 69.56 5 0 0 1300.62 61.74 5 0 0 1209.22 52.55 5 0 0 1451.61 42.40 -5 0 0 1249.30 39.67 -5 0 0 1293.28 50.12 5 0 0 1384.98 41.00 -5 0 0 1422.58 43.32 -6 0 0 205.82 18.59 6 0 0 179.68 25.33 -6 0 0 271.07 33.02 -6 0 0 173.66 20.67 6 0 0 179.48 17.19 -6 0 0 142.60 14.73 6 0 0 160.28 21.37 6 0 0 230.78 18.59 -7 0 0 539.48 33.34 7 0 0 556.46 46.93 -7 0 0 523.00 30.64 -7 0 0 469.59 35.85 7 0 0 623.77 33.90 7 0 0 491.75 40.67 7 0 0 564.63 31.07 -8 0 0 345.66 45.53 8 0 0 370.39 41.67 -8 0 0 367.33 30.40 8 0 0 351.90 27.85 -8 0 0 254.69 23.62 -8 0 0 349.48 33.24 8 0 0 261.44 31.46 8 0 0 422.38 29.21 -9 0 0 31.94 10.11 9 0 0 33.73 10.46 -9 0 0 51.53 17.24 9 0 0 17.82 11.94 -9 0 0 27.25 11.80 9 0 0 25.37 11.02 9 0 0 22.73 9.58 -9 0 0 37.09 10.48 -10 0 0 26.44 10.91 10 0 0 30.07 10.67 -10 0 0 28.66 19.88 10 0 0 38.27 17.40 10 0 0 45.06 16.53 -10 0 0 21.80 10.56 10 0 0 35.02 10.11 -10 0 0 29.92 8.88 -11 0 0 6.59 6.24 11 0 0 4.00 4.65 -11 0 0 0.62 9.12 11 0 0 8.38 9.81 -11 0 0 2.90 3.95 -12 0 0 8.07 6.65 12 0 0 7.61 8.93 -12 0 0 5.04 5.76 -12 0 0 5.33 5.76 -12 0 0 2.69 2.35 12 0 0 3.79 5.31 13 0 0 46.38 13.85 -13 0 0 21.32 11.17 -13 0 0 17.08 17.75 13 0 0 20.85 12.56 -13 0 0 31.16 14.41 -13 0 0 21.67 9.60 -14 0 0 8.75 9.40 14 0 0 9.37 8.09 -14 0 0 1.09 3.43 -14 0 0 6.77 8.05 -14 0 0 6.75 6.63 -15 0 0 -7.55 7.32 15 0 0 -4.83 11.36 -15 0 0 3.15 4.81 -15 0 0 6.56 6.75 -16 0 0 32.26 17.65 16 0 0 42.90 22.64 -16 0 0 29.16 14.87 17 0 0 16.79 17.34 -17 0 0 6.64 10.28 -17 0 0 29.36 15.45 -18 0 0 20.69 12.50 19 0 0 22.33 24.86 -19 0 0 49.29 24.02 -19 0 0 24.52 17.05 20 0 0 -13.80 15.09 -20 0 0 -5.82 9.68 -20 0 0 10.66 9.95 21 0 0 60.51 30.20 -21 0 0 40.56 25.07 22 0 0 4.39 13.47 -22 0 0 -4.68 8.38 -22 0 0 -3.86 9.07 23 0 0 68.58 38.05 -24 0 0 23.75 19.61 0 -1 0 -0.09 1.60 0 1 0 -0.50 1.96 0 1 0 1.52 1.27 0 -1 0 1.08 0.31 0 -1 0 0.17 0.71 1 1 0 180.78 18.76 -1 1 0 162.48 15.98 1 -1 0 166.69 15.32 -1 -1 0 160.93 18.81 -1 1 0 161.66 19.28 1 1 0 190.84 18.37 -1 -1 0 143.18 14.00 -1 1 0 130.84 12.20 1 -1 0 168.41 13.28 1 -1 0 153.62 7.70 1 1 0 156.31 8.53 -1 -1 0 167.22 8.83 -2 -1 0 964.14 44.93 2 1 0 613.73 33.41 -2 1 0 784.15 37.60 -2 1 0 802.58 23.62 2 1 0 809.92 20.33 -2 1 0 656.78 29.33 -2 -1 0 771.04 17.59 2 -1 0 750.31 21.43 2 -1 0 820.15 31.42 -2 -1 0 848.42 24.36 2 1 0 743.85 22.56 -3 -1 0 271.46 25.77 3 1 0 221.27 21.89 -3 1 0 211.41 13.45 -3 1 0 269.98 25.28 3 -1 0 198.18 20.14 3 -1 0 195.11 12.96 3 -1 0 222.61 18.55 3 1 0 194.24 11.96 -3 -1 0 191.78 10.94 -3 1 0 217.88 19.10 -3 1 0 218.56 14.31 -3 -1 0 195.79 13.53 3 -1 0 209.20 9.78 3 1 0 219.96 14.30 -4 1 0 672.70 43.77 4 -1 0 598.29 38.67 -4 1 0 510.10 24.88 -4 -1 0 559.36 40.90 4 1 0 660.33 41.51 4 1 0 474.37 21.80 4 -1 0 618.42 25.99 -4 -1 0 593.92 22.80 -4 1 0 582.78 33.89 -4 1 0 569.78 26.15 4 -1 0 629.44 36.80 4 1 0 567.29 26.55 -4 -1 0 484.40 23.89 4 -1 0 760.55 23.20 5 1 0 109.05 18.84 -5 1 0 131.47 22.26 -5 -1 0 139.73 23.10 -5 1 0 85.84 11.42 5 -1 0 88.38 16.12 5 -1 0 96.56 11.50 -5 1 0 110.56 12.80 -5 1 0 108.33 16.25 5 1 0 102.51 12.20 -5 -1 0 96.22 11.04 5 -1 0 99.52 15.85 -5 -1 0 96.20 14.72 5 -1 0 92.43 9.37 -5 -1 0 94.06 12.24 -6 1 0 21.40 6.50 -6 -1 0 14.91 5.13 6 -1 0 30.95 5.96 6 1 0 22.44 6.23 6 1 0 32.02 11.66 6 -1 0 17.07 8.77 -6 -1 0 17.37 9.69 -6 1 0 19.59 10.10 -6 1 0 24.83 7.54 6 -1 0 29.20 10.09 -6 -1 0 28.47 8.65 -6 -1 0 21.68 5.56 -6 1 0 22.58 6.01 6 -1 0 26.39 6.69 6 1 0 19.40 5.84 7 1 0 180.70 30.02 -7 1 0 156.25 19.36 -7 -1 0 234.70 34.58 7 -1 0 158.28 26.71 -7 -1 0 193.84 23.13 -7 1 0 155.00 21.44 -7 1 0 152.25 17.61 7 1 0 204.89 19.81 7 -1 0 205.54 19.66 -7 -1 0 176.40 17.28 7 -1 0 176.54 25.60 7 1 0 218.23 20.44 7 -1 0 214.98 17.53 -7 -1 0 195.90 20.19 8 -1 0 467.92 49.96 8 1 0 536.23 49.73 -8 -1 0 599.88 58.25 -8 1 0 529.11 55.80 -8 -1 0 485.34 34.62 -8 1 0 499.22 38.67 8 1 0 668.39 37.92 -8 1 0 545.71 43.03 -8 -1 0 383.89 27.49 -8 -1 0 582.45 42.21 8 -1 0 556.22 49.25 -8 1 0 531.94 35.79 8 -1 0 394.80 29.24 8 -1 0 659.26 33.62 8 1 0 715.33 40.07 -9 1 0 69.06 15.15 -9 -1 0 61.33 13.58 9 1 0 57.78 13.66 9 -1 0 56.04 19.64 -9 1 0 84.75 24.67 -9 -1 0 104.79 27.79 9 1 0 60.34 18.80 -9 -1 0 60.69 15.76 -9 1 0 70.89 16.32 9 -1 0 42.69 14.97 -9 -1 0 46.13 10.79 9 -1 0 109.82 15.23 9 -1 0 59.21 12.34 9 1 0 62.90 13.11 -10 -1 0 38.00 11.63 10 -1 0 48.83 10.32 10 1 0 51.17 12.10 -10 1 0 31.69 11.82 -10 1 0 36.70 16.17 10 -1 0 39.38 16.17 -10 -1 0 81.49 25.02 10 -1 0 22.11 13.86 -10 1 0 44.41 13.76 -10 -1 0 34.27 11.98 10 -1 0 32.41 9.47 -10 1 0 44.16 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13.58 14.30 15 0 -21 -45.12 40.38 14 0 -21 17.48 22.94 13 0 -21 -3.59 7.29 13 0 -21 -17.82 26.82 12 0 -21 -13.41 12.43 12 0 -21 -3.13 4.79 11 0 -21 2.61 7.54 11 0 -21 1.51 9.98 10 0 -21 26.07 29.51 7 0 -21 10.52 18.70 6 0 -21 -19.32 26.23 6 0 -21 -0.63 2.22 5 0 -21 16.41 23.27 5 0 -21 33.93 25.30 4 0 -21 -0.55 2.75 4 0 -21 -2.37 19.59 3 0 -21 4.08 12.47 3 0 -21 6.59 19.89 2 0 -21 0.96 11.66 2 0 -21 -1.61 7.18 1 0 -21 -3.49 11.73 17 1 -21 -15.00 11.28 16 1 -21 2.89 8.49 16 -1 -21 4.48 7.74 15 1 -21 1.95 6.78 15 -1 -21 4.65 13.27 15 1 -21 -1.72 11.34 15 -1 -21 2.06 18.58 14 -1 -21 9.77 6.32 14 1 -21 20.92 14.83 14 1 -21 -14.81 35.47 14 -1 -21 -29.47 27.03 13 1 -21 -2.10 9.11 13 1 -21 11.34 22.76 13 -1 -21 -19.83 26.46 12 1 -21 -1.78 4.21 12 1 -21 -2.05 25.26 12 -1 -21 4.49 15.83 11 -1 -21 12.29 14.09 11 1 -21 9.95 10.11 11 -1 -21 -4.28 6.66 11 1 -21 9.56 8.89 10 -1 -21 -12.15 13.70 10 -1 -21 2.46 5.54 10 1 -21 -2.70 10.87 9 -1 -21 -6.05 2.67 9 -1 -21 -16.12 24.86 8 -1 -21 -32.61 32.57 8 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-0.96 8.48 8 -2 -21 -5.11 16.88 8 -2 -21 -5.23 20.15 -7 2 21 -26.29 41.44 7 -2 -21 -18.90 22.12 7 -2 -21 16.68 21.86 6 -2 -21 10.07 18.53 6 -2 -21 14.66 24.74 5 -2 -21 13.53 18.32 5 2 -21 1.75 19.80 5 -2 -21 0.37 12.26 4 -2 -21 -20.67 19.17 4 -2 -21 11.70 2.58 4 2 -21 -0.25 12.07 4 2 -21 20.48 22.01 4 2 -21 11.17 24.26 3 2 -21 -24.09 25.01 3 -2 -21 -18.05 24.48 3 2 -21 14.18 10.39 2 2 -21 4.61 10.85 2 2 -21 -15.72 19.04 2 2 -21 2.91 12.23 1 2 -21 -5.99 7.75 1 2 -21 0.29 11.79 0 2 -21 -12.82 14.63 18 3 -21 -3.00 8.59 16 3 -21 -7.90 6.05 -16 3 21 -194.34 105.22 15 3 -21 -7.74 6.63 -15 3 21 -129.09 114.47 14 3 -21 3.45 2.35 14 3 -21 5.31 13.61 13 3 -21 8.42 6.03 13 3 -21 -19.04 17.12 13 -3 -21 -17.63 20.73 12 3 -21 13.89 14.01 12 3 -21 6.59 15.50 12 -3 -21 -30.67 23.65 11 -3 -21 8.07 13.43 11 3 -21 11.52 13.96 11 3 -21 -11.03 17.85 11 -3 -21 6.43 23.04 11 3 -21 44.87 38.41 -10 3 21 13.93 14.04 10 -3 -21 4.88 11.80 10 3 -21 -7.14 13.57 10 3 -21 6.06 10.88 10 3 -21 6.72 20.10 10 -3 -21 -8.01 16.71 -9 3 21 -26.54 120.45 9 -3 -21 2.98 9.57 9 3 -21 20.70 19.13 9 3 -21 -1.88 12.37 9 -3 -21 16.77 23.38 9 3 -21 -38.55 36.57 8 -3 -21 16.26 19.23 8 3 -21 -11.04 12.47 8 -3 -21 22.60 20.18 8 3 -21 7.93 14.57 8 3 -21 39.87 33.02 7 -3 -21 0.27 17.30 7 -3 -21 14.74 15.25 7 3 -21 22.76 17.84 -6 3 21 -35.27 50.67 6 -3 -21 -15.62 15.61 6 -3 -21 -8.67 3.76 6 3 -21 5.17 13.51 5 3 -21 18.26 19.62 5 -3 -21 34.49 23.42 5 3 -21 -20.30 14.36 4 3 -21 -1.06 7.36 4 3 -21 -18.17 22.38 4 3 -21 1.30 5.50 3 3 -21 0.56 11.85 3 3 -21 -18.79 22.49 2 3 -21 15.22 17.63 2 3 -21 10.70 7.34 2 3 -21 -1.66 2.37 1 3 -21 -1.88 9.38 1 3 -21 -15.36 12.61 0 3 -21 6.01 7.20 -1 3 -21 36.22 25.04 19 4 -21 0.82 0.72 -17 4 21 -78.29 81.22 -16 4 21 113.39 118.24 -15 4 21 269.23 69.11 -14 4 21 -38.66 101.37 -13 4 21 -76.40 97.29 -12 4 21 -49.59 117.95 12 4 -21 -25.42 32.42 -11 4 21 75.16 139.37 11 4 -21 6.62 4.02 11 4 -21 17.97 21.88 -10 4 21 79.03 118.20 10 4 -21 -29.15 21.28 10 4 -21 16.62 30.39 -9 4 21 -34.28 104.24 9 4 -21 -1.29 10.42 9 4 -21 -1.88 4.42 9 4 -21 -8.83 9.38 8 4 -21 -6.47 12.04 8 4 -21 89.89 47.53 7 4 -21 -3.43 9.20 7 4 -21 26.28 13.97 6 4 -21 0.98 7.62 6 4 -21 -0.70 8.58 5 4 -21 -15.06 14.00 5 4 -21 2.63 10.62 5 4 -21 22.58 22.61 4 4 -21 1.95 7.86 4 4 -21 -5.77 17.02 4 4 -21 6.97 10.69 3 4 -21 -18.27 19.34 3 4 -21 43.47 24.86 2 4 -21 33.74 22.52 2 4 -21 3.41 7.21 1 4 -21 5.39 4.76 1 4 -21 22.21 21.56 0 4 -21 14.93 15.08 -1 4 -21 25.75 15.23 -17 5 21 -38.55 61.07 -16 5 21 -165.56 162.85 16 5 -21 3.54 3.57 15 5 -21 -16.87 17.14 -14 5 21 135.77 143.87 -13 5 21 46.08 137.96 -12 5 21 18.08 108.25 -11 5 21 113.50 142.69 -10 5 21 4.91 32.65 10 5 -21 11.44 16.30 10 5 -21 -0.42 23.30 -9 5 21 -33.75 94.92 9 5 -21 -15.02 25.14 -8 5 21 115.95 130.76 8 5 -21 0.38 11.81 -7 5 21 3.09 48.74 7 5 -21 -7.58 14.85 6 5 -21 11.83 10.76 6 5 -21 7.75 8.86 6 5 -21 9.17 11.74 5 5 -21 0.12 6.27 5 5 -21 4.74 2.06 4 5 -21 61.00 34.77 4 5 -21 -38.70 21.46 3 5 -21 20.00 22.02 3 5 -21 -13.24 8.91 3 5 -21 21.15 20.88 2 5 -21 40.77 29.77 2 5 -21 -13.71 8.93 1 5 -21 17.05 15.71 -12 6 21 177.07 154.28 -11 6 21 -130.63 145.71 -10 6 21 13.54 58.17 -9 6 21 -160.28 155.36 -8 6 21 10.19 59.89 8 6 -21 -36.72 31.96 -7 6 21 -39.93 24.66 7 6 -21 -79.60 51.73 -6 6 21 85.24 72.63 6 6 -21 -13.89 18.64 5 6 -21 32.72 31.07 15 0 -22 16.97 12.84 14 0 -22 5.41 2.85 13 0 -22 0.69 7.78 12 0 -22 13.50 24.59 11 0 -22 -9.40 14.37 10 0 -22 -10.14 19.46 10 0 -22 29.26 30.53 9 0 -22 -1.10 15.51 9 0 -22 5.03 16.44 8 0 -22 -20.68 25.99 8 0 -22 6.94 19.61 7 0 -22 9.29 21.40 7 0 -22 -8.31 10.75 6 0 -22 22.05 20.71 6 0 -22 2.84 10.90 5 0 -22 22.75 22.11 16 1 -22 -18.56 16.52 15 1 -22 1.97 10.93 14 -1 -22 18.08 18.42 13 1 -22 14.58 4.39 13 -1 -22 -28.89 23.63 12 -1 -22 17.05 15.42 12 1 -22 6.25 7.21 11 -1 -22 3.99 8.68 11 1 -22 16.86 24.81 11 -1 -22 23.32 20.07 11 1 -22 -16.55 18.47 10 -1 -22 5.43 12.84 10 1 -22 -13.71 20.85 10 1 -22 11.62 16.63 10 -1 -22 -29.06 32.90 9 1 -22 7.32 11.98 9 -1 -22 -8.20 12.32 9 -1 -22 -9.58 2.42 9 1 -22 21.41 20.73 8 -1 -22 -11.58 13.89 8 1 -22 10.21 23.48 8 -1 -22 9.51 22.45 8 1 -22 -18.67 20.51 7 -1 -22 -0.76 8.87 7 1 -22 0.66 6.99 7 1 -22 9.18 17.80 6 1 -22 11.26 13.63 6 1 -22 -10.45 18.44 5 1 -22 -3.90 25.58 5 1 -22 29.33 28.37 4 1 -22 7.95 15.96 17 2 -22 0.41 2.53 16 2 -22 17.09 13.56 15 2 -22 -8.45 11.31 14 2 -22 2.83 9.49 12 2 -22 -27.13 25.00 11 -2 -22 15.60 19.98 11 2 -22 -7.32 3.73 11 2 -22 -28.07 24.21 10 2 -22 -12.76 17.42 10 2 -22 -3.30 13.65 9 2 -22 -14.47 15.20 9 2 -22 20.54 16.73 8 2 -22 -9.10 6.77 8 2 -22 -6.43 4.62 7 2 -22 0.31 9.88 7 2 -22 20.36 22.67 6 2 -22 18.07 17.56 6 2 -22 -17.33 23.61 6 2 -22 14.53 27.41 5 2 -22 -13.34 5.14 5 2 -22 26.51 29.08 4 2 -22 19.42 17.26 4 2 -22 9.90 14.75 3 2 -22 20.59 18.79 18 3 -22 -0.21 6.51 17 3 -22 12.55 9.19 16 3 -22 -7.99 7.27 13 3 -22 0.28 10.45 12 3 -22 18.94 10.81 12 3 -22 9.32 19.32 11 3 -22 -10.96 9.92 11 3 -22 -2.79 8.55 10 3 -22 1.67 12.60 10 3 -22 -10.10 11.60 9 3 -22 21.86 12.05 9 3 -22 -4.77 3.96 9 3 -22 -2.03 15.13 8 3 -22 20.10 12.80 8 3 -22 -1.45 5.12 8 3 -22 -17.52 22.13 7 3 -22 30.27 22.14 7 3 -22 -12.88 20.35 7 3 -22 -18.17 25.91 6 3 -22 4.45 12.62 6 3 -22 11.94 6.26 6 3 -22 19.42 20.45 5 3 -22 -10.52 16.58 5 3 -22 -15.37 23.38 4 3 -22 16.59 19.24 4 3 -22 -24.56 25.28 3 3 -22 0.24 7.46 14 4 -22 15.70 19.25 13 4 -22 0.53 10.53 12 4 -22 8.09 16.47 11 4 -22 -22.11 17.03 10 4 -22 14.79 17.19 9 4 -22 -0.27 20.12 8 4 -22 9.97 16.87 8 4 -22 -14.28 6.80 7 4 -22 -21.04 16.77 7 4 -22 -7.79 10.84 6 4 -22 -9.54 14.46 6 4 -22 14.69 18.67 4 4 -22 8.40 10.63 3 4 -22 29.95 19.95 14 5 -22 40.13 27.02 13 5 -22 -6.26 12.87 12 5 -22 8.03 4.34 11 5 -22 8.55 21.66 10 5 -22 -8.40 4.27 9 5 -22 -29.99 20.44 8 5 -22 29.66 26.11 7 5 -22 -16.26 21.21 4 5 -22 -6.02 10.56 13 0 -23 -11.77 3.94 15 1 -23 -9.85 14.67 14 1 -23 -2.37 11.50 16 2 -23 4.92 4.46 7 2 -23 -22.00 24.82 6 2 -23 11.55 14.83 5 2 -23 26.23 22.10 10 3 -23 15.01 16.02 9 3 -23 34.08 35.09 7 3 -23 -8.01 8.58 6 3 -23 -13.84 21.99 5 3 -23 -33.00 22.47 6 4 -23 4.32 4.55 8 2 -24 -16.77 7.18 8 3 -24 -34.20 19.25 0 0 0 0.00 0.00 TITL DM_SKP3_37 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 17.567853 7.584029 16.119362 90.0000 112.0220 90.0000 ZERR 9.00 0.002276 0.000571 0.002146 0.0000 0.0145 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 27797 _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 8.031 _oxdiff_exptl_absorpt_empirical_full_min 0.327