data_4 _audit_creation_date 2016-12-17 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2013-2 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C19 H24 N2 O2 S' _chemical_formula_sum 'C19 H24 N2 O2 S' _chemical_formula_weight 344.46 _chemical_absolute_configuration syn _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' 'S' 'S' 0.1246 0.1234 '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 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0611(4) _cell_length_b 6.7430(3) _cell_length_c 13.0444(5) _cell_angle_alpha 90 _cell_angle_beta 102.392(3) _cell_angle_gamma 90 _cell_volume 950.25(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4189 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.145 _cell_measurement_theta_min 3.198 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1309 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.8028. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.244 _exptl_crystal_size_mid 0.184 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8891 _diffrn_reflns_point_group_measured_fraction_full 0.903 _diffrn_reflns_point_group_measured_fraction_max 0.890 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.479 _diffrn_reflns_theta_min 2.194 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type bruker-CCD _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.641 _reflns_Friedel_fraction_full 0.789 _reflns_Friedel_fraction_max 0.761 _reflns_number_gt 3508 _reflns_number_total 3877 _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 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.179 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Flack x determined using 1279 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 221 _refine_ls_number_reflns 3877 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0399 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.0524P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.1074 _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 Ternary CH refined with riding coordinates: C2(H2A) 2.b Aromatic/amide H refined with riding coordinates: N2(H2), C15(H15), C13(H13), C5(H5), C14(H14), C11(H11), C12(H12), C9(H9), C6(H6), C7(H7), C8(H8) 2.c Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 S1 S 0.51973(5) 0.23747(10) 0.71545(5) 0.04874(18) Uani 1 1 d . . . . . N2 N 0.31542(17) 0.7734(3) 0.75271(16) 0.0473(5) Uani 1 1 d . . . . . H2 H 0.3734 0.8600 0.7688 0.057 Uiso 1 1 calc R . . . . C10 C 0.2108(2) 0.7856(4) 0.79587(17) 0.0459(6) Uani 1 1 d . . . . . C1 C 0.4589(2) 0.6100(4) 0.6650(2) 0.0454(5) Uani 1 1 d . . . . . O1 O 0.48976(17) 0.7849(3) 0.62935(17) 0.0592(5) Uani 1 1 d . . . . . N1 N 0.53800(18) 0.4708(4) 0.68122(16) 0.0480(5) Uani 1 1 d . . . . . C16 C 0.6204(2) 0.2482(6) 0.8480(2) 0.0625(7) Uani 1 1 d . . . . . C2 C 0.3260(2) 0.6146(4) 0.6809(2) 0.0461(5) Uani 1 1 d . . . . . H2A H 0.3096 0.4890 0.7132 0.055 Uiso 1 1 calc R . . . . O2 O 0.39392(18) 0.1909(3) 0.73170(18) 0.0648(6) Uani 1 1 d . . . . . C3 C 0.6083(3) 0.7979(5) 0.6003(3) 0.0698(9) Uani 1 1 d . . . . . H3A H 0.6120 0.7023 0.5465 0.105 Uiso 1 1 calc GR . . . . H3B H 0.6731 0.7715 0.6606 0.105 Uiso 1 1 calc GR . . . . H3C H 0.6188 0.9287 0.5744 0.105 Uiso 1 1 calc GR . . . . C4 C 0.2364(2) 0.6315(5) 0.5734(2) 0.0578(7) Uani 1 1 d . . . . . C18 C 0.6236(4) 0.0332(8) 0.8872(3) 0.0934(13) Uani 1 1 d . . . . . H18A H 0.5411 -0.0092 0.8886 0.140 Uiso 1 1 calc GR . . . . H18B H 0.6745 0.0254 0.9567 0.140 Uiso 1 1 calc GR . . . . H18C H 0.6573 -0.0510 0.8410 0.140 Uiso 1 1 calc GR . . . . C15 C 0.1830(3) 0.9662(5) 0.8371(2) 0.0570(7) Uani 1 1 d . . . . . H15 H 0.2329 1.0760 0.8339 0.068 Uiso 1 1 calc R . . . . C13 C 0.0058(3) 0.8228(8) 0.8882(3) 0.0847(13) Uani 1 1 d . . . . . H13 H -0.0626 0.8350 0.9185 0.102 Uiso 1 1 calc R . . . . C17 C 0.7477(3) 0.3152(7) 0.8383(3) 0.0900(14) Uani 1 1 d . . . . . H17A H 0.7737 0.2396 0.7845 0.135 Uiso 1 1 calc GR . . . . H17B H 0.8051 0.2954 0.9039 0.135 Uiso 1 1 calc GR . . . . H17C H 0.7452 0.4534 0.8202 0.135 Uiso 1 1 calc GR . . . . C5 C 0.1733(3) 0.4654(7) 0.5299(3) 0.0832(12) Uani 1 1 d . . . . . H5 H 0.1848 0.3438 0.5643 0.100 Uiso 1 1 calc R . . . . C14 C 0.0809(3) 0.9835(7) 0.8830(2) 0.0751(10) Uani 1 1 d . . . . . H14 H 0.0633 1.1048 0.9104 0.090 Uiso 1 1 calc R . . . . C11 C 0.1337(3) 0.6256(6) 0.8009(2) 0.0659(8) Uani 1 1 d . . . . . H11 H 0.1492 0.5040 0.7725 0.079 Uiso 1 1 calc R . . . . C12 C 0.0328(3) 0.6467(8) 0.8486(3) 0.0859(12) Uani 1 1 d . . . . . H12 H -0.0170 0.5374 0.8532 0.103 Uiso 1 1 calc R . . . . C9 C 0.2175(3) 0.8108(7) 0.5210(3) 0.0761(10) Uani 1 1 d . . . . . H9 H 0.2591 0.9234 0.5511 0.091 Uiso 1 1 calc R . . . . C6 C 0.0892(4) 0.4848(12) 0.4300(4) 0.116(2) Uani 1 1 d . . . . . H6 H 0.0444 0.3758 0.3988 0.139 Uiso 1 1 calc R . . . . C19 C 0.5616(4) 0.3845(9) 0.9157(3) 0.1001(15) Uani 1 1 d . . . . . H19A H 0.5618 0.5180 0.8902 0.150 Uiso 1 1 calc GR . . . . H19B H 0.6079 0.3787 0.9869 0.150 Uiso 1 1 calc GR . . . . H19C H 0.4780 0.3431 0.9130 0.150 Uiso 1 1 calc GR . . . . C7 C 0.0756(4) 0.6658(14) 0.3811(4) 0.125(3) Uani 1 1 d . . . . . H7 H 0.0216 0.6779 0.3161 0.150 Uiso 1 1 calc R . . . . C8 C 0.1373(4) 0.8239(10) 0.4242(3) 0.1052(17) Uani 1 1 d . . . . . H8 H 0.1266 0.9446 0.3890 0.126 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0473(3) 0.0419(3) 0.0577(3) -0.0018(3) 0.0127(2) -0.0026(3) N2 0.0392(9) 0.0477(15) 0.0585(10) -0.0067(10) 0.0184(8) -0.0090(9) C10 0.0368(10) 0.0614(19) 0.0401(10) 0.0048(11) 0.0092(8) 0.0012(10) C1 0.0416(11) 0.0424(14) 0.0560(13) -0.0037(11) 0.0188(10) -0.0056(10) O1 0.0511(9) 0.0466(12) 0.0897(13) 0.0068(10) 0.0365(9) -0.0032(8) N1 0.0416(10) 0.0474(13) 0.0582(11) -0.0005(11) 0.0176(9) -0.0046(9) C16 0.0518(13) 0.083(2) 0.0527(12) 0.0043(18) 0.0118(10) -0.0023(17) C2 0.0361(10) 0.0427(14) 0.0638(13) -0.0060(12) 0.0199(10) -0.0065(10) O2 0.0496(10) 0.0459(13) 0.0978(14) 0.0041(10) 0.0136(9) -0.0104(8) C3 0.0621(16) 0.064(2) 0.097(2) 0.0076(17) 0.0482(16) -0.0069(14) C4 0.0397(12) 0.074(2) 0.0642(15) -0.0179(16) 0.0219(11) -0.0034(13) C18 0.086(2) 0.109(3) 0.081(2) 0.031(2) 0.0095(19) 0.002(2) C15 0.0552(14) 0.0672(19) 0.0504(13) 0.0027(14) 0.0157(11) 0.0110(14) C13 0.0547(17) 0.138(4) 0.0696(19) 0.017(2) 0.0323(15) 0.016(2) C17 0.0459(15) 0.135(4) 0.083(2) 0.017(2) 0.0011(14) -0.0119(18) C5 0.0497(15) 0.104(3) 0.101(2) -0.053(2) 0.0269(16) -0.0192(18) C14 0.0727(19) 0.099(3) 0.0590(16) 0.0071(18) 0.0257(15) 0.031(2) C11 0.0537(15) 0.077(2) 0.0740(17) -0.0046(17) 0.0296(13) -0.0154(15) C12 0.0553(17) 0.122(4) 0.089(2) 0.007(2) 0.0363(17) -0.018(2) C9 0.0667(18) 0.098(3) 0.0634(18) 0.0011(18) 0.0136(14) -0.0010(17) C6 0.059(2) 0.179(6) 0.112(4) -0.084(4) 0.025(2) -0.029(3) C19 0.094(3) 0.141(4) 0.066(2) -0.030(2) 0.0173(18) 0.006(3) C7 0.070(3) 0.231(9) 0.074(3) -0.037(4) 0.0124(19) -0.004(4) C8 0.083(3) 0.162(5) 0.065(2) 0.009(3) 0.0026(18) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 N1 1.659(2) . ? S1 C16 1.846(3) . ? S1 O2 1.485(2) . ? N2 H2 0.8600 . ? N2 C10 1.394(3) . ? N2 C2 1.444(3) . ? C10 C15 1.391(4) . ? C10 C11 1.386(4) . ? C1 O1 1.339(3) . ? C1 N1 1.270(3) . ? C1 C2 1.527(3) . ? O1 C3 1.444(3) . ? C16 C18 1.536(7) . ? C16 C17 1.509(4) . ? C16 C19 1.515(5) . ? C2 H2A 0.9800 . ? C2 C4 1.537(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.377(5) . ? C4 C9 1.383(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C15 H15 0.9300 . ? C15 C14 1.392(4) . ? C13 H13 0.9300 . ? C13 C14 1.375(6) . ? C13 C12 1.354(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C5 H5 0.9300 . ? C5 C6 1.436(7) . ? C14 H14 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.397(4) . ? C12 H12 0.9300 . ? C9 H9 0.9300 . ? C9 C8 1.381(5) . ? C6 H6 0.9300 . ? C6 C7 1.370(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C7 H7 0.9300 . ? C7 C8 1.324(9) . ? C8 H8 0.9300 . ? 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 N1 S1 C16 97.52(15) . . ? O2 S1 N1 114.24(11) . . ? O2 S1 C16 105.67(12) . . ? C10 N2 H2 120.1 . . ? C10 N2 C2 119.8(2) . . ? C2 N2 H2 120.1 . . ? C15 C10 N2 118.7(2) . . ? C11 C10 N2 123.1(3) . . ? C11 C10 C15 118.3(2) . . ? O1 C1 C2 110.7(2) . . ? N1 C1 O1 119.4(2) . . ? N1 C1 C2 129.9(2) . . ? C1 O1 C3 117.3(2) . . ? C1 N1 S1 128.77(18) . . ? C18 C16 S1 104.0(3) . . ? C17 C16 S1 108.6(2) . . ? C17 C16 C18 110.8(3) . . ? C17 C16 C19 113.1(4) . . ? C19 C16 S1 108.8(2) . . ? C19 C16 C18 111.1(3) . . ? N2 C2 C1 108.50(19) . . ? N2 C2 H2A 108.2 . . ? N2 C2 C4 114.2(2) . . ? C1 C2 H2A 108.2 . . ? C1 C2 C4 109.2(2) . . ? C4 C2 H2A 108.2 . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 119.1(3) . . ? C5 C4 C9 119.8(3) . . ? C9 C4 C2 121.0(3) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C15 H15 119.8 . . ? C10 C15 C14 120.4(3) . . ? C14 C15 H15 119.8 . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C12 C13 C14 119.2(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C5 H5 120.9 . . ? C4 C5 C6 118.2(5) . . ? C6 C5 H5 120.9 . . ? C15 C14 H14 119.7 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C10 C11 H11 120.0 . . ? C10 C11 C12 120.0(4) . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 121.5(4) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C4 C9 H9 119.7 . . ? C8 C9 C4 120.5(4) . . ? C8 C9 H9 119.7 . . ? C5 C6 H6 120.4 . . ? C7 C6 C5 119.2(5) . . ? C7 C6 H6 120.4 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C6 C7 H7 119.2 . . ? C8 C7 C6 121.7(5) . . ? C8 C7 H7 119.2 . . ? C9 C8 H8 119.7 . . ? C7 C8 C9 120.5(6) . . ? C7 C8 H8 119.7 . . ? 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 N2 C10 C15 C14 -178.6(2) . . . . ? N2 C10 C11 C12 177.8(3) . . . . ? N2 C2 C4 C5 -135.3(3) . . . . ? N2 C2 C4 C9 43.9(3) . . . . ? C10 N2 C2 C1 -167.8(2) . . . . ? C10 N2 C2 C4 70.2(3) . . . . ? C10 C15 C14 C13 -0.1(4) . . . . ? C10 C11 C12 C13 1.7(5) . . . . ? C1 C2 C4 C5 103.0(3) . . . . ? C1 C2 C4 C9 -77.8(3) . . . . ? O1 C1 N1 S1 -174.50(18) . . . . ? O1 C1 C2 N2 -57.4(3) . . . . ? O1 C1 C2 C4 67.6(3) . . . . ? N1 S1 C16 C18 -174.6(2) . . . . ? N1 S1 C16 C17 -56.5(3) . . . . ? N1 S1 C16 C19 66.9(3) . . . . ? N1 C1 O1 C3 6.6(4) . . . . ? N1 C1 C2 N2 122.0(3) . . . . ? N1 C1 C2 C4 -112.9(3) . . . . ? C16 S1 N1 C1 -112.9(2) . . . . ? C2 N2 C10 C15 -160.2(2) . . . . ? C2 N2 C10 C11 20.6(4) . . . . ? C2 C1 O1 C3 -173.9(2) . . . . ? C2 C1 N1 S1 6.1(4) . . . . ? C2 C4 C5 C6 179.4(3) . . . . ? C2 C4 C9 C8 179.6(3) . . . . ? O2 S1 N1 C1 -1.9(3) . . . . ? O2 S1 C16 C18 67.5(2) . . . . ? O2 S1 C16 C17 -174.4(3) . . . . ? O2 S1 C16 C19 -50.9(3) . . . . ? C4 C5 C6 C7 0.7(6) . . . . ? C4 C9 C8 C7 1.3(6) . . . . ? C15 C10 C11 C12 -1.4(4) . . . . ? C5 C4 C9 C8 -1.2(5) . . . . ? C5 C6 C7 C8 -0.6(8) . . . . ? C14 C13 C12 C11 -1.2(6) . . . . ? C11 C10 C15 C14 0.7(4) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C9 C4 C5 C6 0.2(4) . . . . ? C6 C7 C8 C9 -0.4(8) . . . . ? _shelx_res_file ; TITL cxl2016090801MPJdata_0m in P21 #4 REM reset to P21 #4 CELL 0.71073 11.0611 6.743 13.0444 90 102.392 90 ZERR 2 0.0004 0.0003 0.0005 0 0.0025 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 19 24 2 2 1 L.S. 4 PLAN 20 TEMP 23 BOND MORE -1 BOND $H CONF fmap 2 acta 52 REM REM REM WGHT 0.064400 0.052400 FVAR 1.15878 S1 5 0.519732 0.237470 0.715454 11.00000 0.04726 0.04190 = 0.05771 -0.00183 0.01272 -0.00262 N2 3 0.315425 0.773376 0.752708 11.00000 0.03923 0.04774 = 0.05848 -0.00674 0.01836 -0.00902 AFIX 43 H2 2 0.373446 0.860037 0.768805 11.00000 -1.20000 AFIX 0 C10 1 0.210820 0.785647 0.795871 11.00000 0.03678 0.06144 = 0.04006 0.00479 0.00920 0.00120 C1 1 0.458851 0.610042 0.665030 11.00000 0.04163 0.04241 = 0.05601 -0.00370 0.01877 -0.00563 O1 4 0.489762 0.784902 0.629350 11.00000 0.05110 0.04656 = 0.08965 0.00676 0.03645 -0.00318 N1 3 0.537999 0.470754 0.681219 11.00000 0.04158 0.04739 = 0.05824 -0.00046 0.01756 -0.00461 C16 1 0.620442 0.248229 0.847993 11.00000 0.05184 0.08312 = 0.05268 0.00426 0.01185 -0.00233 C2 1 0.326038 0.614629 0.680861 11.00000 0.03608 0.04268 = 0.06377 -0.00597 0.01990 -0.00649 AFIX 13 H2A 2 0.309609 0.489047 0.713155 11.00000 -1.20000 AFIX 0 O2 4 0.393918 0.190950 0.731704 11.00000 0.04962 0.04588 = 0.09781 0.00409 0.01364 -0.01038 C3 1 0.608348 0.797942 0.600296 11.00000 0.06213 0.06434 = 0.09682 0.00758 0.04818 -0.00689 AFIX 137 H3A 2 0.611961 0.702262 0.546538 11.00000 -1.50000 H3B 2 0.673080 0.771532 0.660610 11.00000 -1.50000 H3C 2 0.618839 0.928702 0.574423 11.00000 -1.50000 AFIX 0 C4 1 0.236447 0.631519 0.573439 11.00000 0.03974 0.07440 = 0.06423 -0.01791 0.02194 -0.00343 C18 1 0.623645 0.033205 0.887249 11.00000 0.08617 0.10950 = 0.08076 0.03137 0.00950 0.00170 AFIX 137 H18A 2 0.541150 -0.009194 0.888603 11.00000 -1.50000 H18B 2 0.674523 0.025413 0.956711 11.00000 -1.50000 H18C 2 0.657265 -0.051033 0.840977 11.00000 -1.50000 AFIX 0 C15 1 0.182996 0.966163 0.837051 11.00000 0.05524 0.06717 = 0.05043 0.00271 0.01574 0.01103 AFIX 43 H15 2 0.232930 1.075976 0.833876 11.00000 -1.20000 AFIX 0 C13 1 0.005840 0.822848 0.888185 11.00000 0.05469 0.13834 = 0.06965 0.01733 0.03233 0.01646 AFIX 43 H13 2 -0.062575 0.835049 0.918545 11.00000 -1.20000 AFIX 0 C17 1 0.747665 0.315243 0.838262 11.00000 0.04589 0.13549 = 0.08278 0.01663 0.00105 -0.01190 AFIX 137 H17A 2 0.773662 0.239598 0.784482 11.00000 -1.50000 H17B 2 0.805076 0.295352 0.903933 11.00000 -1.50000 H17C 2 0.745191 0.453411 0.820182 11.00000 -1.50000 AFIX 0 C5 1 0.173301 0.465353 0.529896 11.00000 0.04966 0.10376 = 0.10098 -0.05310 0.02686 -0.01921 AFIX 43 H5 2 0.184835 0.343783 0.564283 11.00000 -1.20000 AFIX 0 C14 1 0.080886 0.983498 0.882984 11.00000 0.07270 0.09873 = 0.05902 0.00708 0.02568 0.03086 AFIX 43 H14 2 0.063276 1.104817 0.910395 11.00000 -1.20000 AFIX 0 C11 1 0.133722 0.625581 0.800897 11.00000 0.05368 0.07720 = 0.07403 -0.00458 0.02965 -0.01544 AFIX 43 H11 2 0.149181 0.504049 0.772528 11.00000 -1.20000 AFIX 0 C12 1 0.032796 0.646749 0.848564 11.00000 0.05526 0.12245 = 0.08938 0.00723 0.03630 -0.01783 AFIX 43 H12 2 -0.016997 0.537397 0.853181 11.00000 -1.20000 AFIX 0 C9 1 0.217491 0.810771 0.520980 11.00000 0.06670 0.09817 = 0.06338 0.00110 0.01360 -0.00100 AFIX 43 H9 2 0.259054 0.923400 0.551091 11.00000 -1.20000 AFIX 0 C6 1 0.089162 0.484790 0.429973 11.00000 0.05912 0.17893 = 0.11188 -0.08353 0.02501 -0.02912 AFIX 43 H6 2 0.044409 0.375753 0.398759 11.00000 -1.20000 AFIX 0 C19 1 0.561634 0.384506 0.915738 11.00000 0.09396 0.14072 = 0.06583 -0.02984 0.01728 0.00619 AFIX 137 H19A 2 0.561812 0.518012 0.890207 11.00000 -1.50000 H19B 2 0.607869 0.378725 0.986929 11.00000 -1.50000 H19C 2 0.477956 0.343138 0.913006 11.00000 -1.50000 AFIX 0 C7 1 0.075564 0.665751 0.381149 11.00000 0.06953 0.23123 = 0.07385 -0.03721 0.01235 -0.00409 AFIX 43 H7 2 0.021616 0.677885 0.316129 11.00000 -1.20000 AFIX 0 C8 1 0.137294 0.823861 0.424190 11.00000 0.08319 0.16179 = 0.06457 0.00877 0.00265 0.00840 AFIX 43 H8 2 0.126571 0.944642 0.388983 11.00000 -1.20000 AFIX 0 HKLF 4 REM cxl2016090801MPJdata_0m in P21 #4 REM R1 = 0.0399 for 3508 Fo > 4sig(Fo) and 0.0449 for all 3877 data REM 221 parameters refined using 1 restraints END WGHT 0.0644 0.0524 REM Highest difference peak 0.179, deepest hole -0.247, 1-sigma level 0.054 Q1 1 0.3300 0.9053 0.7295 11.00000 0.05 0.18 Q2 1 0.0962 0.3463 0.4572 11.00000 0.05 0.16 Q3 1 0.7444 0.5969 0.7213 11.00000 0.05 0.16 Q4 1 0.5011 1.0600 0.5168 11.00000 0.05 0.16 Q5 1 0.5222 0.8920 0.5041 11.00000 0.05 0.16 Q6 1 0.6363 0.8744 0.4430 11.00000 0.05 0.15 Q7 1 0.5189 0.7327 0.5096 11.00000 0.05 0.14 Q8 1 0.7675 0.7667 0.7346 11.00000 0.05 0.14 Q9 1 0.3440 0.3976 0.9109 11.00000 0.05 0.14 Q10 1 0.3196 1.2496 0.8581 11.00000 0.05 0.14 Q11 1 0.3507 0.3755 0.8463 11.00000 0.05 0.14 Q12 1 0.3578 1.0061 0.8812 11.00000 0.05 0.14 Q13 1 0.7346 0.7385 0.7230 11.00000 0.05 0.14 Q14 1 0.4675 0.4931 0.8998 11.00000 0.05 0.14 Q15 1 0.4394 0.0009 0.8737 11.00000 0.05 0.14 Q16 1 0.6035 0.8291 0.4800 11.00000 0.05 0.13 Q17 1 0.8127 0.7149 0.7439 11.00000 0.05 0.13 Q18 1 0.6667 0.7448 0.7469 11.00000 0.05 0.13 Q19 1 0.7045 -0.0972 0.8003 11.00000 0.05 0.13 Q20 1 0.3563 1.1039 0.9172 11.00000 0.05 0.13 ; _shelx_res_checksum 53696 _shelx_hkl_file ; 2 0 0 1809.56 40.53 1 -2 0 0 1795.89 40.47 1 3 0 0 1531.85 35.22 1 -3 0 0 1578.60 37.15 3 -3 0 0 1541.71 35.11 1 4 0 0 261.904 6.720 1 -4 0 0 251.699 6.549 1 -4 0 0 248.759 6.754 3 -4 0 0 249.301 6.858 4 4 0 0 258.189 6.832 4 5 0 0 5.36269 0.79512 1 5 0 0 4.18660 0.58650 4 -5 0 0 5.22066 0.74946 1 -5 0 0 4.31317 0.60930 4 -5 0 0 3.29277 0.59594 3 -6 0 0 196.123 5.676 4 -6 0 0 197.919 5.662 1 -6 0 0 191.712 5.809 3 6 0 0 196.117 5.889 1 -7 0 0 493.294 12.744 1 7 0 0 488.657 13.076 1 -7 0 0 511.849 13.280 4 -7 0 0 506.938 13.398 3 -8 0 0 97.9723 3.9313 3 -8 0 0 95.4687 3.7618 1 -8 0 0 103.403 3.477 4 8 0 0 92.7009 3.9692 1 -9 0 0 4.45401 1.09393 1 -9 0 0 5.89286 1.21107 3 9 0 0 3.53507 1.20500 1 10 0 0 41.6966 2.9704 1 -10 0 0 43.6130 2.8768 3 -10 0 0 37.6504 2.5743 1 -11 0 0 8.37273 1.64502 3 -11 0 0 8.41511 1.53029 1 11 0 0 8.70992 1.80125 1 -12 0 0 -0.3695 0.8611 1 -13 0 0 45.1916 3.1884 1 -14 0 0 26.1407 2.8696 1 0 -1 0 -3.4436 0.2241 2 0 1 0 -2.6808 0.3229 2 1 -1 0 5680.57 163.06 2 -1 1 0 5877.00 161.48 2 -2 -1 0 201.995 6.008 4 -2 1 0 205.263 5.638 3 2 1 0 201.891 5.906 4 2 1 0 201.121 5.103 1 -2 1 0 213.941 6.389 2 -2 1 0 207.366 4.910 1 -3 -1 0 122.584 4.145 4 -3 1 0 130.142 3.392 1 3 1 0 121.928 4.032 4 -3 1 0 125.321 3.901 3 3 1 0 132.713 3.624 1 -4 -1 0 474.615 11.549 1 4 -1 0 487.349 11.602 1 -4 -1 0 448.871 12.842 4 4 1 0 482.346 11.679 1 4 1 0 468.256 12.749 4 -4 1 0 485.281 11.396 1 -4 1 0 477.297 12.396 3 5 -1 0 972.614 22.860 1 -5 -1 0 938.932 25.062 4 -5 -1 0 996.773 22.794 1 -5 1 0 991.814 22.594 1 -5 1 0 949.641 24.248 3 5 1 0 954.358 24.909 4 5 1 0 973.409 22.932 1 -6 -1 0 304.951 9.180 4 -6 -1 0 331.086 8.519 1 -6 -1 0 313.066 8.429 3 6 -1 0 318.235 8.621 1 6 1 0 305.885 9.034 4 -6 1 0 302.808 8.226 1 -6 1 0 322.924 8.294 4 6 1 0 322.038 8.686 1 -6 1 0 319.505 9.085 3 -7 -1 0 608.104 15.116 1 7 -1 0 618.621 15.354 1 -7 -1 0 600.221 15.425 3 -7 -1 0 587.426 16.284 4 -7 1 0 606.361 14.869 1 7 1 0 609.753 16.182 4 7 1 0 574.815 15.266 1 -7 1 0 594.020 16.095 3 -8 -1 0 503.481 13.581 1 8 -1 0 511.969 13.893 1 -8 -1 0 536.037 14.531 4 -8 -1 0 535.025 13.916 3 8 1 0 519.150 13.897 1 -8 1 0 512.451 13.344 1 -8 1 0 512.799 14.562 3 8 1 0 539.101 14.411 4 -9 -1 0 254.533 7.724 1 -9 -1 0 245.957 7.802 4 -9 -1 0 248.817 7.670 3 9 1 0 246.871 7.959 1 9 1 0 260.726 7.828 4 -9 1 0 231.018 7.340 1 -9 1 0 243.213 8.256 3 -10 -1 0 1.89305 0.93466 3 -10 -1 0 1.60795 0.92602 1 10 1 0 2.80767 1.20504 1 -10 1 0 1.76696 1.00269 3 -10 1 0 1.61067 0.87935 1 -11 -1 0 39.2172 2.8098 1 -11 1 0 43.0050 2.6619 1 -11 1 0 45.1739 3.2962 3 11 1 0 38.9795 2.9773 1 12 1 0 60.9551 3.9051 1 -12 1 0 64.0838 3.4098 1 -12 1 0 59.4052 4.1038 3 -13 1 0 13.1181 2.4414 3 13 1 0 12.1851 2.1687 1 -13 1 0 11.0827 1.7977 1 0 -2 0 2519.97 71.35 2 0 2 0 2653.29 71.44 2 0 2 0 2417.39 60.58 3 0 2 0 2519.91 62.88 4 1 -2 0 2011.92 57.74 2 -1 -2 0 2048.41 58.17 2 1 2 0 2043.66 51.23 4 -1 2 0 2066.50 57.91 2 -1 2 0 2050.44 49.34 3 -1 2 0 2052.70 50.92 4 1 2 0 2028.63 49.07 3 2 -2 0 295.535 9.341 2 -2 -2 0 285.974 8.834 4 -2 2 0 306.967 9.642 2 2 2 0 301.642 8.729 4 -2 2 0 293.084 8.238 3 3 -2 0 278.268 8.873 2 -3 -2 0 259.708 8.612 4 -3 2 0 298.701 9.342 2 -3 2 0 281.252 8.106 3 3 2 0 297.435 6.929 1 3 2 0 286.227 8.545 4 3 2 0 288.777 6.962 1 -4 -2 0 743.531 20.770 4 -4 2 0 777.639 17.614 1 -4 2 0 766.135 19.811 3 -4 2 0 773.779 17.631 1 -4 2 0 786.116 22.786 2 4 2 0 754.964 18.064 1 4 2 0 781.166 20.589 4 -5 -2 0 44.0325 2.6203 4 -5 -2 0 53.7251 2.1304 1 -5 2 0 44.2668 1.7175 1 5 2 0 46.1412 2.5284 4 -5 2 0 46.8656 2.4969 2 -5 2 0 47.0717 1.7745 1 5 2 0 44.7843 2.0390 1 -6 -2 0 150.832 5.585 4 -6 -2 0 142.564 4.619 1 -6 2 0 142.043 5.257 3 6 2 0 140.714 5.269 4 -6 2 0 147.033 4.212 1 6 2 0 144.246 4.683 1 -7 -2 0 148.226 5.730 4 7 2 0 149.941 5.063 1 7 2 0 153.960 5.571 4 -7 2 0 147.854 4.512 1 -7 2 0 147.273 5.611 3 -8 -2 0 317.802 8.535 3 -8 -2 0 304.904 9.746 4 -8 2 0 293.373 9.688 3 8 2 0 302.371 8.901 1 -8 2 0 294.495 8.195 1 8 2 0 301.579 9.504 4 -9 -2 0 20.9633 2.3109 4 -9 2 0 20.1033 2.4116 3 9 2 0 19.6675 2.1173 4 9 2 0 23.1630 2.2639 1 -9 2 0 22.3839 1.6611 1 -10 -2 0 109.625 4.904 4 -10 2 0 107.198 4.167 1 10 2 0 105.680 4.767 1 10 2 0 112.686 4.830 4 -10 2 0 116.052 5.449 3 -11 2 0 105.259 4.286 1 -11 2 0 112.408 5.570 3 11 2 0 104.119 4.914 1 -12 2 0 2.37764 1.38215 3 -12 2 0 1.72334 0.97652 1 12 2 0 1.94913 1.24662 1 -13 2 0 2.76119 1.12752 1 13 2 0 2.78789 1.46935 1 -13 2 0 3.84135 1.75373 3 0 -3 0 0.15521 0.53580 2 0 3 0 -0.0735 0.4505 4 0 3 0 0.31662 0.54576 2 0 3 0 -0.4993 0.3754 3 -1 -3 0 85.9377 4.3619 2 1 -3 0 85.4034 4.0741 2 -1 3 0 87.5149 4.2262 2 1 3 0 89.9727 3.7320 4 -1 3 0 83.8602 3.4553 4 -1 3 0 83.6276 3.3901 3 1 3 0 84.6099 3.1885 3 2 -3 0 99.6174 4.2765 2 -2 -3 0 89.7972 4.6974 2 -2 -3 0 97.5955 4.2763 4 -2 3 0 98.4289 4.5067 2 -2 3 0 91.5229 3.5871 4 2 3 0 95.6417 4.0537 4 -3 -3 0 214.258 8.773 2 3 -3 0 228.343 7.784 2 -3 3 0 232.385 8.294 2 -3 3 0 221.427 7.068 3 -3 3 0 220.832 6.760 4 3 3 0 219.141 7.489 4 4 -3 0 19.7703 1.5180 2 -4 -3 0 20.8948 2.3006 4 -4 3 0 21.4789 1.4444 4 -4 3 0 22.0709 1.9511 2 -4 3 0 20.1220 1.7020 3 4 3 0 20.1576 1.8196 4 -5 -3 0 106.968 4.982 4 5 3 0 110.440 3.329 1 5 3 0 103.936 4.670 4 -5 3 0 110.784 4.571 3 5 3 0 113.254 3.319 1 -6 -3 0 72.6083 3.9146 4 -6 3 0 64.1927 1.8752 1 -6 3 0 64.9477 1.8636 1 6 3 0 65.6636 2.5768 1 -6 3 0 56.8725 3.3256 3 6 3 0 62.8677 3.4985 4 -7 -3 0 119.581 5.443 4 7 3 0 123.200 4.156 1 7 3 0 115.953 5.113 4 -7 3 0 114.718 3.379 1 -7 3 0 107.808 5.017 3 -8 -3 0 112.906 5.403 4 -8 3 0 111.536 5.268 3 8 3 0 121.790 5.279 4 8 3 0 110.724 4.300 1 -8 3 0 119.162 3.626 1 -9 -3 0 16.2725 2.2658 4 9 3 0 18.2271 2.2761 4 -9 3 0 16.3972 2.3677 3 9 3 0 15.7494 1.8612 1 -9 3 0 19.4961 1.3582 1 -10 -3 0 29.8064 3.1320 4 10 3 0 26.4732 2.7800 4 10 3 0 23.4989 2.3546 1 -10 3 0 26.0862 1.6955 1 -10 3 0 32.2499 3.4807 3 -11 -3 0 53.7320 3.6783 4 -11 3 0 50.0284 2.5057 1 11 3 0 48.1679 3.1550 1 11 3 0 61.5147 3.6738 4 -11 3 0 53.5812 3.9392 3 12 3 0 8.09211 1.74364 1 -12 3 0 11.7237 1.4685 1 -12 3 0 16.3718 2.7380 3 -13 3 0 9.22212 2.52089 3 13 3 0 7.70858 1.83036 1 -13 3 0 10.2217 1.4616 1 0 -4 0 689.035 22.049 2 0 4 0 681.353 19.092 4 0 4 0 686.271 18.179 3 1 -4 0 513.504 16.959 2 -1 -4 0 498.998 17.380 2 -1 4 0 502.649 14.668 4 1 4 0 511.593 14.994 4 -1 4 0 538.781 14.366 3 1 4 0 513.072 13.932 3 -2 -4 0 296.360 9.965 4 -2 -4 0 285.460 11.226 2 2 -4 0 286.798 10.407 2 -2 4 0 293.984 9.058 3 -2 4 0 298.266 9.081 4 2 4 0 275.974 9.468 4 3 -4 0 252.138 8.876 2 -3 -4 0 232.228 9.924 2 -3 -4 0 242.906 8.860 4 -3 4 0 242.745 7.700 4 3 4 0 239.605 8.438 4 -3 4 0 229.576 7.914 3 -4 -4 0 90.3860 5.4535 2 -4 -4 0 90.2186 4.8011 4 4 -4 0 89.8544 4.2416 2 -4 4 0 94.3275 4.2960 3 -4 4 0 97.0343 3.8397 4 4 4 0 94.6327 4.5817 4 -5 -4 0 74.1887 5.1265 2 -5 -4 0 87.3343 4.7551 4 5 -4 0 81.7621 3.7997 2 -5 4 0 81.6814 4.1222 3 5 4 0 85.1023 4.3918 4 -6 -4 0 118.478 6.854 2 -6 -4 0 108.068 5.617 4 -6 4 0 110.426 5.184 3 6 4 0 118.425 5.433 4 -7 -4 0 166.616 7.470 4 -7 4 0 158.008 6.832 3 7 4 0 178.569 4.680 1 7 4 0 175.595 7.113 4 -8 -4 0 24.6264 3.1571 4 -8 4 0 26.0925 3.0635 3 8 4 0 27.0724 3.0595 4 8 4 0 26.0747 1.7070 1 -9 -4 0 87.3006 5.2437 4 9 4 0 83.4872 4.7840 4 -9 4 0 80.5324 4.8490 3 9 4 0 83.0459 3.4626 1 -10 -4 0 52.5849 4.0426 4 10 4 0 60.1475 3.0604 1 10 4 0 61.2007 4.0490 4 -10 4 0 59.4458 4.2441 3 -11 -4 0 9.48927 2.28172 4 11 4 0 9.75901 1.63054 1 11 4 0 13.0545 2.3030 4 -11 4 0 10.5416 2.3650 3 -12 4 0 -0.9547 1.0882 3 12 4 0 1.63144 1.48107 4 12 4 0 2.84863 1.25982 1 0 -5 0 -0.7452 0.9826 2 0 5 0 -0.0936 0.9650 3 0 5 0 -0.7451 1.0979 4 1 -5 0 166.401 7.581 2 -1 -5 0 151.830 6.758 4 -1 -5 0 155.583 7.819 2 -1 5 0 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381.516 11.270 4 2 2 9 383.679 10.345 1 -2 2 -9 381.872 12.388 4 -2 2 -9 390.370 10.748 1 2 2 9 394.317 10.376 1 -3 -2 -9 20.4654 1.8402 4 3 2 9 20.5019 1.8721 1 -3 2 -9 20.2703 1.9875 1 -3 2 -9 18.9258 2.4102 4 3 2 9 23.9238 1.7871 1 -4 -2 -9 3.60551 1.06655 4 -4 2 -9 4.88832 1.43273 4 -4 2 -9 8.68888 1.39002 1 4 2 9 3.18020 0.97587 1 -5 -2 -9 34.1342 2.4162 4 5 2 9 34.2312 2.3339 1 -5 2 -9 31.0977 2.2715 1 -5 2 -9 33.5704 2.8352 3 -5 2 -9 32.9975 2.8638 4 -6 -2 -9 13.7006 1.8534 4 6 2 9 13.8843 1.8219 1 -6 2 -9 11.5906 2.0773 4 -6 2 -9 13.5757 1.7791 1 -7 -2 -9 28.4826 2.4175 4 7 2 9 33.0124 2.5142 1 -7 2 -9 28.8838 2.3760 1 -7 2 -9 29.5418 3.2533 4 -8 -2 -9 14.1844 2.0755 4 -8 2 -9 18.8326 2.7532 4 8 2 9 10.3746 1.8365 1 -8 2 -9 14.1470 1.9457 1 -9 -2 -9 13.1026 2.0714 4 -9 2 -9 13.7230 2.0100 1 9 2 9 11.3358 2.0106 1 12 3 -9 80.2334 4.6563 1 -12 3 9 72.5579 4.7854 3 -12 3 9 83.1024 3.2196 1 -11 3 9 47.8851 2.3256 1 -11 3 9 46.9523 3.5931 3 11 3 -9 49.1394 3.4736 1 -10 3 9 25.7498 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instructions were received'