data_publication_text _publ_requested_journal 'Acta Chim.Slov.' _publ_contact_author_name 'Goreshnik, Evgeny' _publ_contact_author_address ;Department of Inorganic Chemistry and Technology, Jozef Stefan Institute, Jamova 39, SI-1000 Ljubljana, Slovenia ; _publ_contact_author_email evgeny.goreshnik@ijs.si loop_ _publ_author_name _publ_author_address 'Fedorchuk, Andrii A.' ;Institute of Nuclear Physics Polish Academy of Sciences, Radzikowskiego 152, PL-31342 Krakow, Poland ; 'Goreshnik, Evgeny' ;Department of Inorganic Chemistry and Technology, Jozef Stefan Institute, Jamova 39, SI-1000 Ljubljana, Slovenia ; 'Slyvka, Yurii' ;Department of Inorganic Chemistry, Ivan Franko National University, Kyryla i Mefodia Str, 6, 79005 L'viv, Ukraine ; 'Mys`kiv, Marian' ;Department of Inorganic Chemistry, Ivan Franko National University, Kyryla i Mefodia Str, 6, 79005 L'viv, Ukraine ; data_5623 _audit_creation_date 2020-04-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? loop_ _publ_body_element _publ_body_title _publ_body_contents section ; Introduction ; ; ; section ; Experimental ; ; ; subsection ; Synthesis and crystallization ; ; ; subsection ; Refinement ; ; Crystal data, data collection and structure refinement details are summarized in Table 1. ; section ; Results and discussion ; ; ; _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. 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. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H16 Cu N4 O2 S2, C6 H5 O3 S' _chemical_formula_sum 'C18 H21 Cu N4 O5 S3' _chemical_formula_weight 533.11 _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' 'Cu' 'Cu' 0.3201 1.2651 '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 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1664(6) _cell_length_b 10.7387(6) _cell_length_c 12.4008(6) _cell_angle_alpha 93.096(4) _cell_angle_beta 95.581(5) _cell_angle_gamma 114.254(6) _cell_volume 1101.71(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4336 _cell_measurement_temperature 396(2) _cell_measurement_theta_max 28.2900 _cell_measurement_theta_min 4.2380 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 548 _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.418 _exptl_crystal_size_min 0.343 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0385 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.783 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7786 _diffrn_reflns_point_group_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.783 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.882 _diffrn_reflns_theta_min 3.736 _diffrn_ambient_temperature 396.15 _diffrn_detector_area_resol_mean 5.3213 _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.783 _diffrn_measurement_device_type 'New Gemini, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3954 _reflns_number_total 4534 _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 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _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 1.106 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.078 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 288 _refine_ls_number_reflns 4534 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0376 _refine_ls_restrained_S_all 1.065 _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^)+(0.0365P)^2^+1.2162P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.0912 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2.a Ternary CH refined with riding coordinates: C5A(H5A) 2.b Secondary CH2 refined with riding coordinates: C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB) 2.c Aromatic/amide H refined with riding coordinates: N2A(H2A), N2B(H2B), C5B(H5B), C23(H23), C33(H33), C43(H43), C53(H53), C63(H63) 2.d X=CH2 refined with riding coordinates: C6B(H6BA,H6BB) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _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 Cu1 Cu 0.64957(4) 0.93467(3) 0.50087(2) 0.02032(10) Uani 1 1 d . . . . . S1 S 0.40192(8) 0.81070(6) 0.54657(5) 0.01781(15) Uani 1 1 d . . . . . S2 S 0.66864(9) 0.88998(7) 0.32425(5) 0.02267(16) Uani 1 1 d . . . . . O1A O 0.6124(3) 0.9422(2) 0.94359(15) 0.0311(5) Uani 1 1 d . . . . . O1B O 0.6234(3) 0.4567(2) 0.12801(16) 0.0296(5) Uani 1 1 d . . . . . N1A N 0.5534(3) 0.8901(2) 0.75717(16) 0.0157(4) Uani 1 1 d . . . . . N1B N 0.6491(3) 0.6687(2) 0.20053(16) 0.0165(4) Uani 1 1 d . . . . . N2A N 0.2881(3) 0.8037(2) 0.73665(17) 0.0194(5) Uani 1 1 d . . . . . H2A H 0.189801 0.765368 0.705669 0.023 Uiso 1 1 calc R . . . . N2B N 0.6273(3) 0.6354(2) 0.37202(17) 0.0192(5) Uani 1 1 d . . . . . H2B H 0.617875 0.649336 0.439428 0.023 Uiso 1 1 calc R . . . . C1A C 0.4151(3) 0.8358(2) 0.68338(19) 0.0150(5) Uani 1 1 d . . . . . C1B C 0.6466(3) 0.7267(3) 0.30229(19) 0.0149(5) Uani 1 1 d . . . . . C2A C 0.5148(3) 0.8978(3) 0.8631(2) 0.0203(6) Uani 1 1 d . . . . . C2B C 0.6318(3) 0.5345(3) 0.2048(2) 0.0193(5) Uani 1 1 d . . . . . C3A C 0.3335(3) 0.8402(3) 0.8527(2) 0.0243(6) Uani 1 1 d . . . . . H3AA H 0.289698 0.760415 0.892488 0.029 Uiso 1 1 calc R . . . . H3AB H 0.297731 0.908535 0.878573 0.029 Uiso 1 1 calc R . . . . C3B C 0.6235(3) 0.5083(3) 0.3227(2) 0.0202(5) Uani 1 1 d . . . . . H3BA H 0.524597 0.430364 0.331624 0.024 Uiso 1 1 calc R . . . . H3BB H 0.715215 0.492546 0.353271 0.024 Uiso 1 1 calc R . . . . C4A C 0.7197(3) 0.9349(3) 0.7346(2) 0.0194(5) Uani 1 1 d . . . . . H4AA H 0.735484 0.855584 0.707227 0.023 Uiso 1 1 calc R . . . . H4AB H 0.791919 0.974478 0.802044 0.023 Uiso 1 1 calc R . . . . C4B C 0.6705(4) 0.7391(3) 0.1008(2) 0.0229(6) Uani 1 1 d . . . . . H4BA H 0.605304 0.791027 0.097000 0.027 Uiso 1 1 calc R . . . . H4BB H 0.633041 0.671278 0.037732 0.027 Uiso 1 1 calc R . . . . C5A C 0.7628(3) 1.0385(3) 0.65328(19) 0.0173(5) Uani 1 1 d . . . . . H5A H 0.747562 1.121742 0.672307 0.021 Uiso 1 1 calc R . . . . C5B C 0.8453(4) 0.8353(3) 0.0977(2) 0.0277(6) Uani 1 1 d . . . . . H5B H 0.894800 0.906467 0.153465 0.033 Uiso 1 1 calc R . . . . C6A C 0.8787(3) 1.0537(3) 0.5879(2) 0.0227(6) Uani 1 1 d . . . . . H6AA H 0.917(4) 1.128(3) 0.551(2) 0.020(7) Uiso 1 1 d . . . . . H6AB H 0.932(4) 0.992(3) 0.590(2) 0.026(8) Uiso 1 1 d . . . . . C6B C 0.9312(4) 0.8260(3) 0.0233(3) 0.0364(7) Uani 1 1 d . . . . . H6BA H 0.885940 0.756140 -0.033768 0.044 Uiso 1 1 calc R . . . . H6BB H 1.038203 0.889071 0.026901 0.044 Uiso 1 1 calc R . . . . S3 S 0.86425(8) 0.65840(7) 0.61328(5) 0.02094(15) Uani 1 1 d . . . . . O13 O 0.7078(2) 0.6645(2) 0.59626(14) 0.0230(4) Uani 1 1 d . . . . . C13 C 0.8488(3) 0.5370(3) 0.7080(2) 0.0199(5) Uani 1 1 d . . . . . C23 C 0.7724(4) 0.5380(3) 0.7986(2) 0.0265(6) Uani 1 1 d . . . . . H23 H 0.720914 0.596134 0.806267 0.032 Uiso 1 1 calc R . . . . C33 C 0.7728(4) 0.4519(4) 0.8781(2) 0.0371(8) Uani 1 1 d . . . . . H33 H 0.719880 0.450709 0.938629 0.045 Uiso 1 1 calc R . . . . C43 C 0.8522(4) 0.3682(3) 0.8669(3) 0.0381(8) Uani 1 1 d . . . . . H43 H 0.854386 0.311886 0.920793 0.046 Uiso 1 1 calc R . . . . C53 C 0.9287(4) 0.3673(3) 0.7761(3) 0.0328(7) Uani 1 1 d . . . . . H53 H 0.982189 0.310624 0.769492 0.039 Uiso 1 1 calc R . . . . C63 C 0.9257(3) 0.4505(3) 0.6948(2) 0.0246(6) Uani 1 1 d . . . . . H63 H 0.974329 0.448391 0.632730 0.030 Uiso 1 1 calc R . . . . O23 O 0.9092(3) 0.6126(2) 0.51519(17) 0.0354(5) Uani 1 1 d . . . A 1 O33 O 0.9867(2) 0.7874(2) 0.66787(19) 0.0351(5) Uani 1 1 d . . . B 1 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 Cu1 0.02233(19) 0.02390(19) 0.01283(16) -0.00126(12) 0.00249(12) 0.00812(15) S1 0.0186(3) 0.0183(3) 0.0138(3) 0.0007(2) -0.0029(2) 0.0061(3) S2 0.0408(4) 0.0164(3) 0.0142(3) 0.0026(2) 0.0065(3) 0.0146(3) O1A 0.0325(12) 0.0541(14) 0.0144(9) 0.0002(9) -0.0004(9) 0.0271(11) O1B 0.0423(13) 0.0207(10) 0.0243(10) -0.0046(8) 0.0039(9) 0.0125(10) N1A 0.0175(11) 0.0215(11) 0.0111(9) 0.0028(8) 0.0016(8) 0.0111(9) N1B 0.0232(12) 0.0138(10) 0.0113(9) 0.0015(8) 0.0033(8) 0.0065(9) N2A 0.0171(11) 0.0205(11) 0.0200(11) 0.0053(9) 0.0027(9) 0.0070(9) N2B 0.0276(13) 0.0181(11) 0.0139(10) 0.0065(8) 0.0088(9) 0.0095(10) C1A 0.0186(13) 0.0115(11) 0.0165(12) 0.0047(9) 0.0001(10) 0.0079(10) C1B 0.0154(12) 0.0170(12) 0.0122(11) 0.0027(9) 0.0033(9) 0.0061(10) C2A 0.0261(14) 0.0271(14) 0.0157(12) 0.0062(11) 0.0054(11) 0.0180(12) C2B 0.0205(13) 0.0153(13) 0.0202(12) 0.0015(10) 0.0019(11) 0.0056(11) C3A 0.0271(15) 0.0321(16) 0.0198(13) 0.0095(11) 0.0085(11) 0.0166(13) C3B 0.0246(14) 0.0137(12) 0.0217(13) 0.0046(10) 0.0075(11) 0.0061(11) C4A 0.0174(13) 0.0305(15) 0.0138(11) 0.0011(10) -0.0012(10) 0.0143(12) C4B 0.0344(16) 0.0233(14) 0.0113(11) 0.0034(10) 0.0023(11) 0.0124(13) C5A 0.0169(13) 0.0179(13) 0.0144(11) -0.0041(10) -0.0038(10) 0.0065(11) C5B 0.0355(17) 0.0253(15) 0.0201(13) 0.0070(11) 0.0074(12) 0.0092(13) C6A 0.0212(14) 0.0248(15) 0.0204(13) 0.0035(11) 0.0013(11) 0.0080(12) C6B 0.0390(19) 0.0363(18) 0.0315(16) 0.0057(14) 0.0097(14) 0.0119(16) S3 0.0161(3) 0.0245(3) 0.0248(3) 0.0077(3) 0.0062(3) 0.0097(3) O13 0.0197(10) 0.0364(11) 0.0178(9) 0.0068(8) 0.0047(7) 0.0157(9) C13 0.0156(13) 0.0191(13) 0.0220(13) 0.0010(10) -0.0010(10) 0.0051(11) C23 0.0274(15) 0.0313(16) 0.0234(14) 0.0011(12) 0.0040(12) 0.0152(13) C33 0.044(2) 0.050(2) 0.0230(15) 0.0102(14) 0.0102(14) 0.0235(17) C43 0.050(2) 0.0387(18) 0.0308(16) 0.0135(14) 0.0029(15) 0.0231(17) C53 0.0394(18) 0.0242(15) 0.0376(17) 0.0009(13) -0.0005(14) 0.0175(14) C63 0.0223(14) 0.0247(15) 0.0266(14) 0.0006(11) 0.0043(12) 0.0095(12) O23 0.0385(13) 0.0518(14) 0.0311(11) 0.0159(10) 0.0197(10) 0.0295(12) O33 0.0231(11) 0.0273(11) 0.0534(14) 0.0063(10) -0.0014(10) 0.0101(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 Cu1 S1 2.2573(8) . ? Cu1 S2 2.2556(7) . ? Cu1 C5A 2.081(2) . ? Cu1 C6A 2.101(3) . ? S1 C1A 1.688(2) . ? S2 C1B 1.684(3) . ? O1A C2A 1.203(3) . ? O1B C2B 1.207(3) . ? N1A C1A 1.376(3) . ? N1A C2A 1.400(3) . ? N1A C4A 1.459(3) . ? N1B C1B 1.383(3) . ? N1B C2B 1.388(3) . ? N1B C4B 1.472(3) . ? N2A H2A 0.8600 . ? N2A C1A 1.325(3) . ? N2A C3A 1.445(3) . ? N2B H2B 0.8600 . ? N2B C1B 1.311(3) . ? N2B C3B 1.451(3) . ? C2A C3A 1.505(4) . ? C2B C3B 1.507(3) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C3B H3BA 0.9700 . ? C3B H3BB 0.9700 . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? C4A C5A 1.500(4) . ? C4B H4BA 0.9700 . ? C4B H4BB 0.9700 . ? C4B C5B 1.514(4) . ? C5A H5A 0.9800 . ? C5A C6A 1.361(4) . ? C5B H5B 0.9300 . ? C5B C6B 1.295(4) . ? C6A H6AA 0.90(3) . ? C6A H6AB 0.97(3) . ? C6B H6BA 0.9300 . ? C6B H6BB 0.9300 . ? S3 O13 1.4578(19) . ? S3 C13 1.774(3) . ? S3 O23 1.446(2) . ? S3 O33 1.453(2) . ? C13 C23 1.382(4) . ? C13 C63 1.390(4) . ? C23 H23 0.9300 . ? C23 C33 1.389(4) . ? C33 H33 0.9300 . ? C33 C43 1.378(5) . ? C43 H43 0.9300 . ? C43 C53 1.385(5) . ? C53 H53 0.9300 . ? C53 C63 1.388(4) . ? C63 H63 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 S2 Cu1 S1 112.97(3) . . ? C5A Cu1 S1 98.58(8) . . ? C5A Cu1 S2 148.39(8) . . ? C5A Cu1 C6A 37.96(11) . . ? C6A Cu1 S1 135.03(8) . . ? C6A Cu1 S2 110.77(8) . . ? C1A S1 Cu1 107.20(9) . . ? C1B S2 Cu1 108.99(9) . . ? C1A N1A C2A 110.3(2) . . ? C1A N1A C4A 127.6(2) . . ? C2A N1A C4A 122.1(2) . . ? C1B N1B C2B 110.9(2) . . ? C1B N1B C4B 125.2(2) . . ? C2B N1B C4B 123.9(2) . . ? C1A N2A H2A 123.9 . . ? C1A N2A C3A 112.3(2) . . ? C3A N2A H2A 123.9 . . ? C1B N2B H2B 123.8 . . ? C1B N2B C3B 112.4(2) . . ? C3B N2B H2B 123.8 . . ? N1A C1A S1 127.3(2) . . ? N2A C1A S1 123.65(19) . . ? N2A C1A N1A 109.1(2) . . ? N1B C1B S2 122.26(18) . . ? N2B C1B S2 129.02(19) . . ? N2B C1B N1B 108.7(2) . . ? O1A C2A N1A 124.5(3) . . ? O1A C2A C3A 129.4(2) . . ? N1A C2A C3A 106.1(2) . . ? O1B C2B N1B 125.8(2) . . ? O1B C2B C3B 128.4(2) . . ? N1B C2B C3B 105.8(2) . . ? N2A C3A C2A 102.2(2) . . ? N2A C3A H3AA 111.3 . . ? N2A C3A H3AB 111.3 . . ? C2A C3A H3AA 111.3 . . ? C2A C3A H3AB 111.3 . . ? H3AA C3A H3AB 109.2 . . ? N2B C3B C2B 102.01(19) . . ? N2B C3B H3BA 111.4 . . ? N2B C3B H3BB 111.4 . . ? C2B C3B H3BA 111.4 . . ? C2B C3B H3BB 111.4 . . ? H3BA C3B H3BB 109.2 . . ? N1A C4A H4AA 109.0 . . ? N1A C4A H4AB 109.0 . . ? N1A C4A C5A 112.8(2) . . ? H4AA C4A H4AB 107.8 . . ? C5A C4A H4AA 109.0 . . ? C5A C4A H4AB 109.0 . . ? N1B C4B H4BA 109.3 . . ? N1B C4B H4BB 109.3 . . ? N1B C4B C5B 111.7(2) . . ? H4BA C4B H4BB 107.9 . . ? C5B C4B H4BA 109.3 . . ? C5B C4B H4BB 109.3 . . ? Cu1 C5A H5A 115.5 . . ? C4A C5A Cu1 107.41(17) . . ? C4A C5A H5A 115.5 . . ? C6A C5A Cu1 71.81(15) . . ? C6A C5A C4A 122.6(2) . . ? C6A C5A H5A 115.5 . . ? C4B C5B H5B 117.5 . . ? C6B C5B C4B 124.9(3) . . ? C6B C5B H5B 117.5 . . ? Cu1 C6A H6AA 103.2(19) . . ? Cu1 C6A H6AB 103.9(19) . . ? C5A C6A Cu1 70.23(16) . . ? C5A C6A H6AA 120.6(19) . . ? C5A C6A H6AB 119.5(19) . . ? H6AA C6A H6AB 119(3) . . ? C5B C6B H6BA 120.0 . . ? C5B C6B H6BB 120.0 . . ? H6BA C6B H6BB 120.0 . . ? O13 S3 C13 106.91(12) . . ? O23 S3 O13 113.18(12) . . ? O23 S3 C13 107.54(13) . . ? O23 S3 O33 113.44(14) . . ? O33 S3 O13 110.60(12) . . ? O33 S3 C13 104.54(13) . . ? C23 C13 S3 119.4(2) . . ? C23 C13 C63 121.1(3) . . ? C63 C13 S3 119.3(2) . . ? C13 C23 H23 120.2 . . ? C13 C23 C33 119.7(3) . . ? C33 C23 H23 120.2 . . ? C23 C33 H33 120.2 . . ? C43 C33 C23 119.6(3) . . ? C43 C33 H33 120.2 . . ? C33 C43 H43 119.7 . . ? C33 C43 C53 120.7(3) . . ? C53 C43 H43 119.7 . . ? C43 C53 H53 119.9 . . ? C43 C53 C63 120.3(3) . . ? C63 C53 H53 119.9 . . ? C13 C63 H63 120.6 . . ? C53 C63 C13 118.7(3) . . ? C53 C63 H63 120.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2A H2A S3 0.86 2.81 3.671(2) 175.1 1_455 yes N2A H2A O33 0.86 1.99 2.743(3) 146.0 1_455 yes N2B H2B S3 0.86 2.93 3.456(2) 121.0 . yes N2B H2B O13 0.86 2.01 2.774(3) 147.8 . yes C3A H3AB O1A 0.97 2.51 3.202(3) 128.4 2_677 yes C3B H3BA O13 0.97 2.25 3.137(3) 151.6 2_666 yes C3B H3BB O23 0.97 2.45 3.146(4) 128.5 . yes C4A H4AA O13 0.97 2.32 3.249(3) 160.7 . yes C4B H4BA O1A 0.97 2.56 3.170(3) 121.4 1_554 yes C63 H63 O23 0.93 2.40 3.309(4) 165.7 2_766 yes 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 Cu1 S1 C1A N1A -15.5(2) . . . . ? Cu1 S1 C1A N2A 164.94(18) . . . . ? Cu1 S2 C1B N1B 178.54(18) . . . . ? Cu1 S2 C1B N2B -2.4(3) . . . . ? O1A C2A C3A N2A -179.2(3) . . . . ? O1B C2B C3B N2B -175.6(3) . . . . ? N1A C2A C3A N2A 0.6(3) . . . . ? N1A C4A C5A Cu1 -73.6(2) . . . . ? N1A C4A C5A C6A -152.8(2) . . . . ? N1B C2B C3B N2B 3.6(3) . . . . ? N1B C4B C5B C6B 119.8(3) . . . . ? C1A N1A C2A O1A -179.4(3) . . . . ? C1A N1A C2A C3A 0.8(3) . . . . ? C1A N1A C4A C5A 54.8(3) . . . . ? C1A N2A C3A C2A -1.8(3) . . . . ? C1B N1B C2B O1B 177.0(3) . . . . ? C1B N1B C2B C3B -2.2(3) . . . . ? C1B N1B C4B C5B 77.7(3) . . . . ? C1B N2B C3B C2B -4.2(3) . . . . ? C2A N1A C1A S1 178.44(18) . . . . ? C2A N1A C1A N2A -2.0(3) . . . . ? C2A N1A C4A C5A -125.5(2) . . . . ? C2B N1B C1B S2 178.76(19) . . . . ? C2B N1B C1B N2B -0.4(3) . . . . ? C2B N1B C4B C5B -101.0(3) . . . . ? C3A N2A C1A S1 -177.98(18) . . . . ? C3A N2A C1A N1A 2.4(3) . . . . ? C3B N2B C1B S2 -176.1(2) . . . . ? C3B N2B C1B N1B 3.0(3) . . . . ? C4A N1A C1A S1 -1.9(4) . . . . ? C4A N1A C1A N2A 177.7(2) . . . . ? C4A N1A C2A O1A 0.9(4) . . . . ? C4A N1A C2A C3A -178.9(2) . . . . ? C4A C5A C6A Cu1 99.4(2) . . . . ? C4B N1B C1B S2 -0.1(4) . . . . ? C4B N1B C1B N2B -179.2(2) . . . . ? C4B N1B C2B O1B -4.1(4) . . . . ? C4B N1B C2B C3B 176.7(2) . . . . ? S3 C13 C23 C33 -174.1(2) . . . . ? S3 C13 C63 C53 172.6(2) . . . . ? O13 S3 C13 C23 -43.4(3) . . . . ? O13 S3 C13 C63 142.1(2) . . . . ? C13 C23 C33 C43 1.3(5) . . . . ? C23 C13 C63 C53 -1.8(4) . . . . ? C23 C33 C43 C53 -1.3(5) . . . . ? C33 C43 C53 C63 -0.2(5) . . . . ? C43 C53 C63 C13 1.8(4) . . . . ? C63 C13 C23 C33 0.3(4) . . . . ? O23 S3 C13 C23 -165.2(2) . . . . ? O23 S3 C13 C63 20.2(3) . . . . ? O33 S3 C13 C23 73.9(2) . . . . ? O33 S3 C13 C63 -100.6(2) . . . . ? _shelx_res_file ; TITL 5623_a.res in P-1 5623.res created by SHELXL-2018/3 at 23:51:32 on 03-Apr-2020 REM Old TITL 5623 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.101, Rweak 0.007, Alpha 0.056, Orientation as input REM Formula found by SHELXT: C5A N4 O6 S3 Cu CELL 0.71073 9.166412 10.738707 12.40084 93.0956 95.5811 114.2539 ZERR 2 0.000594 0.000608 0.000553 0.0041 0.0045 0.0058 LATT 1 SFAC C H Cu N O S UNIT 36 42 2 8 10 6 EQIV $1 -1+X,+Y,+Z EQIV $2 1-X,2-Y,2-Z EQIV $3 1-X,1-Y,1-Z EQIV $4 +X,+Y,-1+Z EQIV $5 2-X,1-Y,1-Z L.S. 10 PLAN 5 TEMP 123 HTAB N2A S3_$1 HTAB N2A O33_$1 HTAB N2B S3 HTAB N2B O13 HTAB C3A O1A_$2 HTAB C3B O13_$3 HTAB C3B O23 HTAB C4A O13 HTAB C4B O1A_$4 HTAB C63 O23_$5 HTAB BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.036500 1.216200 FVAR 6.09648 CU1 3 0.649574 0.934670 0.500873 11.00000 0.02233 0.02390 = 0.01283 -0.00126 0.00249 0.00812 S1 6 0.401921 0.810700 0.546568 11.00000 0.01858 0.01825 = 0.01376 0.00074 -0.00286 0.00608 S2 6 0.668643 0.889982 0.324255 11.00000 0.04075 0.01636 = 0.01424 0.00256 0.00646 0.01456 O1A 5 0.612426 0.942234 0.943590 11.00000 0.03254 0.05411 = 0.01443 0.00015 -0.00042 0.02714 O1B 5 0.623438 0.456701 0.128006 11.00000 0.04226 0.02072 = 0.02430 -0.00462 0.00390 0.01253 N1A 4 0.553351 0.890141 0.757168 11.00000 0.01746 0.02151 = 0.01105 0.00281 0.00157 0.01111 N1B 4 0.649081 0.668707 0.200534 11.00000 0.02324 0.01384 = 0.01128 0.00153 0.00325 0.00652 N2A 4 0.288087 0.803660 0.736648 11.00000 0.01714 0.02052 = 0.01998 0.00530 0.00270 0.00698 AFIX 43 H2A 2 0.189801 0.765368 0.705669 11.00000 -1.20000 AFIX 0 N2B 4 0.627266 0.635439 0.372016 11.00000 0.02761 0.01806 = 0.01387 0.00647 0.00876 0.00949 AFIX 43 H2B 2 0.617875 0.649336 0.439428 11.00000 -1.20000 AFIX 0 C1A 1 0.415113 0.835827 0.683384 11.00000 0.01861 0.01147 = 0.01647 0.00465 0.00007 0.00785 C1B 1 0.646579 0.726720 0.302292 11.00000 0.01542 0.01701 = 0.01216 0.00268 0.00332 0.00613 C2A 1 0.514815 0.897789 0.863141 11.00000 0.02609 0.02706 = 0.01570 0.00620 0.00540 0.01797 C2B 1 0.631759 0.534491 0.204788 11.00000 0.02050 0.01526 = 0.02020 0.00150 0.00195 0.00561 C3A 1 0.333508 0.840244 0.852707 11.00000 0.02712 0.03213 = 0.01976 0.00954 0.00848 0.01662 AFIX 23 H3AA 2 0.289698 0.760415 0.892488 11.00000 -1.20000 H3AB 2 0.297731 0.908535 0.878573 11.00000 -1.20000 AFIX 0 C3B 1 0.623506 0.508306 0.322696 11.00000 0.02464 0.01371 = 0.02168 0.00462 0.00753 0.00610 AFIX 23 H3BA 2 0.524597 0.430364 0.331624 11.00000 -1.20000 H3BB 2 0.715215 0.492546 0.353271 11.00000 -1.20000 AFIX 0 C4A 1 0.719697 0.934876 0.734617 11.00000 0.01736 0.03048 = 0.01380 0.00114 -0.00120 0.01428 AFIX 23 H4AA 2 0.735484 0.855584 0.707227 11.00000 -1.20000 H4AB 2 0.791919 0.974478 0.802044 11.00000 -1.20000 AFIX 0 C4B 1 0.670489 0.739123 0.100789 11.00000 0.03438 0.02335 = 0.01132 0.00343 0.00229 0.01244 AFIX 23 H4BA 2 0.605304 0.791027 0.097000 11.00000 -1.20000 H4BB 2 0.633041 0.671278 0.037732 11.00000 -1.20000 AFIX 0 C5A 1 0.762813 1.038511 0.653276 11.00000 0.01685 0.01794 = 0.01436 -0.00413 -0.00385 0.00650 AFIX 13 H5A 2 0.747562 1.121742 0.672307 11.00000 -1.20000 AFIX 0 C5B 1 0.845344 0.835307 0.097708 11.00000 0.03555 0.02528 = 0.02006 0.00698 0.00740 0.00921 AFIX 43 H5B 2 0.894800 0.906467 0.153465 11.00000 -1.20000 AFIX 0 C6A 1 0.878718 1.053680 0.587949 11.00000 0.02122 0.02476 = 0.02044 0.00345 0.00133 0.00803 H6AA 2 0.917297 1.127738 0.550702 11.00000 0.02031 H6AB 2 0.931523 0.991537 0.589823 11.00000 0.02618 C6B 1 0.931239 0.825960 0.023283 11.00000 0.03901 0.03627 = 0.03151 0.00574 0.00972 0.01190 AFIX 93 H6BA 2 0.885940 0.756140 -0.033768 11.00000 -1.20000 H6BB 2 1.038203 0.889071 0.026901 11.00000 -1.20000 AFIX 0 S3 6 0.864245 0.658404 0.613276 11.00000 0.01613 0.02446 = 0.02482 0.00767 0.00618 0.00971 O13 5 0.707773 0.664454 0.596262 11.00000 0.01967 0.03640 = 0.01780 0.00684 0.00475 0.01568 C13 1 0.848826 0.536988 0.708047 11.00000 0.01559 0.01912 = 0.02200 0.00104 -0.00096 0.00506 C23 1 0.772382 0.538038 0.798622 11.00000 0.02743 0.03130 = 0.02345 0.00113 0.00396 0.01517 AFIX 43 H23 2 0.720914 0.596134 0.806267 11.00000 -1.20000 AFIX 0 C33 1 0.772818 0.451912 0.878145 11.00000 0.04391 0.05028 = 0.02301 0.01016 0.01023 0.02351 AFIX 43 H33 2 0.719880 0.450709 0.938629 11.00000 -1.20000 AFIX 0 C43 1 0.852169 0.368250 0.866881 11.00000 0.05005 0.03866 = 0.03077 0.01354 0.00292 0.02313 AFIX 43 H43 2 0.854386 0.311886 0.920793 11.00000 -1.20000 AFIX 0 C53 1 0.928667 0.367267 0.776056 11.00000 0.03942 0.02420 = 0.03756 0.00085 -0.00045 0.01755 AFIX 43 H53 2 0.982189 0.310624 0.769492 11.00000 -1.20000 AFIX 0 C63 1 0.925743 0.450477 0.694829 11.00000 0.02227 0.02468 = 0.02664 0.00057 0.00429 0.00954 AFIX 43 H63 2 0.974329 0.448391 0.632730 11.00000 -1.20000 AFIX 0 PART 1 O23 5 0.909195 0.612624 0.515187 11.00000 0.03854 0.05179 = 0.03107 0.01585 0.01973 0.02952 O33 5 0.986672 0.787433 0.667868 11.00000 0.02305 0.02730 = 0.05344 0.00631 -0.00142 0.01010 HKLF 4 REM 5623_a.res in P-1 REM wR2 = 0.0912, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0376 for 3954 Fo > 4sig(Fo) and 0.0460 for all 4534 data REM 288 parameters refined using 0 restraints END WGHT 0.0365 1.2160 REM Instructions for potential hydrogen bonds HTAB N2A S3_$1 HTAB N2A O33_$1 HTAB N2B S3 HTAB N2B O13 HTAB C3A O1A_$2 HTAB C3B O13_$3 HTAB C3B O23 HTAB C4A O13 HTAB C4B O1A_$4 HTAB C63 O23_$5 REM Highest difference peak 1.106, deepest hole -0.653, 1-sigma level 0.078 Q1 1 0.9063 0.6923 0.6802 11.00000 0.05 1.11 Q2 1 0.9562 0.7892 0.7485 11.00000 0.05 0.57 Q3 1 0.9834 0.6754 0.5804 11.00000 0.05 0.57 Q4 1 0.7874 0.7710 0.0545 11.00000 0.05 0.44 Q5 1 0.6173 0.5214 0.2603 11.00000 0.05 0.38 ; _shelx_res_checksum 41478 _shelx_hkl_file ; 0 0 -3 10432.3 483.069 2 0 0 -3 10944.9 402.654 1 0 0 3 10999.2 364.187 1 0 0 4 420.879 111.851 1 0 0 -4 474.406 134.234 1 0 0 -4 570.565 183.850 2 0 0 -5 221439. 3274.60 1 0 0 5 224344. 3321.84 2 0 0 -5 217094. 3636.18 2 0 0 5 224001. 2978.65 1 0 0 6 96244.5 1955.04 2 0 0 -6 93108.1 2260.69 2 0 0 -6 95032.0 1948.31 1 0 0 6 96106.2 1640.36 1 0 0 -7 44296.4 1614.75 2 0 0 7 46612.5 1072.05 1 0 0 7 46054.5 1321.04 2 0 0 8 33105.7 909.748 1 0 0 8 35482.3 1189.72 2 0 0 -8 33292.2 1507.16 2 0 0 9 4098.84 422.553 3 0 0 -9 4365.28 611.260 2 0 0 9 4975.69 459.351 2 0 0 -10 44515.1 1987.44 2 0 0 10 40112.2 1381.39 3 0 0 11 70937.5 1495.93 1 0 0 11 71475.2 1938.44 3 0 0 -11 70224.3 2659.17 2 0 0 -12 987.267 499.179 2 0 0 12 1962.92 340.382 3 0 0 12 1489.04 203.198 1 0 0 13 2834.88 416.874 3 0 0 -13 2988.22 688.575 2 0 0 13 2725.09 265.939 1 0 0 -14-432.254 528.607 2 0 0 14 758.017 294.301 3 0 0 -15 507.176 479.363 2 0 0 -16 22469.8 1751.89 2 0 1 -16 19332.5 1703.87 2 0 1 -15 15832.7 1566.35 2 0 -1 14 2459.13 365.972 3 0 1 -14 2027.20 659.280 2 0 -1 13 19511.4 689.426 1 0 -1 13 21664.6 1008.61 3 0 1 -13 21089.1 1673.56 2 0 -1 12 42996.9 1427.45 3 0 -1 12 43109.8 1100.74 1 0 1 -12 44316.8 2304.87 2 0 1 -11 29514.3 1797.51 2 0 -1 11 28867.3 1172.64 2 0 -1 11 25417.3 1055.42 3 0 -1 10 35918.0 1341.32 2 0 1 -10 34218.4 1849.87 2 0 -1 10 34486.1 1200.47 3 0 -1 9 3422.99 420.195 2 0 1 -9 2627.80 509.844 2 0 -1 9 2783.13 272.038 1 0 -1 9 2992.85 356.652 3 0 -1 8 33539.7 918.548 1 0 -1 8 32358.7 1067.59 3 0 -1 8 31361.5 1197.45 2 0 1 -8 30864.3 1550.10 2 0 -1 7 38417.0 1110.25 3 0 -1 7 39903.8 985.956 1 0 1 -7 38506.3 1633.96 2 0 -1 7 38579.8 1299.50 2 0 -1 6 8740.21 430.070 1 0 1 -6 7981.34 687.747 2 0 -1 6 8871.28 476.460 3 0 -1 6 9005.69 584.946 2 0 -1 5 47975.3 1097.98 3 0 -1 5 47016.6 1049.61 1 0 1 -5 44333.4 1535.98 2 0 1 -4 25758.1 1052.67 2 0 -1 4 26875.0 714.017 3 0 -1 3 3717.22 230.671 3 0 1 -3 3736.18 226.239 3 0 1 -3 3991.30 393.783 2 0 -1 2 7590.04 273.113 3 0 1 -2 7414.33 456.600 2 0 -1 -3 31375.5 787.634 2 0 -1 -3 30072.0 745.964 1 0 -1 -4 393359. 5059.82 2 0 1 4 390925. 4732.91 1 0 -1 -4 392033. 4925.08 1 0 -1 -5 282185. 4145.80 2 0 -1 -5 280162. 3915.67 1 0 1 5 286718. 3684.98 1 0 -1 -6 87635.0 1840.97 1 0 -1 -6 87803.8 2055.13 2 0 1 6 88646.4 1583.53 1 0 -1 -7 12485.7 781.126 2 0 -1 -7 12281.3 679.297 1 0 1 7 12807.7 533.739 1 0 -1 -8 823.534 298.627 2 0 1 8 655.137 143.376 1 0 -1 -8 818.954 269.367 1 0 -1 -9 60312.8 1807.32 1 0 -1 -9 61979.0 2071.08 2 0 -1 -10 4814.46 534.689 1 0 -1 -10 5010.28 665.207 2 0 1 10 4572.75 354.470 1 0 -1 -11 11690.0 1042.72 2 0 1 11 10812.7 536.098 1 0 1 12 106839. 2669.36 3 0 1 12 105020. 1927.14 1 0 -1 -13 8168.23 990.570 2 0 1 13 7853.22 456.106 1 0 1 13 6962.99 665.057 3 0 -1 -14 2897.90 664.484 2 0 1 14 2424.41 423.270 3 0 -1 -15 38.6287 462.712 2 0 -1 -16-777.057 519.376 2 0 2 -16 5928.12 1111.74 2 0 2 -15 1948.85 666.631 2 0 2 -14 31392.6 2203.58 2 0 2 -13 126258. 4387.75 2 0 -2 13 125847. 2579.18 3 0 -2 12 27517.2 1065.04 3 0 2 -12 27740.2 1917.23 2 0 -2 11 86260.3 1996.31 3 0 2 -11 85704.0 3278.89 2 0 -2 10 7544.96 538.608 3 0 2 -10 7437.21 941.939 2 0 -2 10 7357.98 645.292 2 0 -2 9 72.8428 182.943 2 0 -2 9 15.2613 133.526 3 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136.028 1 -1 4 -2 373.552 299.671 2 -1 4 -3 12025.3 958.594 2 1 -4 3 11056.1 473.130 1 -1 4 -3 10818.2 466.909 3 1 -4 4 1666.83 217.410 3 -1 4 -4 1658.18 488.901 2 -1 4 -4 2117.70 221.318 3 1 -4 5 24902.5 768.850 3 -1 4 -5 26460.8 723.442 3 -1 4 -5 24898.4 1500.61 2 -1 4 -6 1204.68 170.166 3 1 -4 6 1020.95 162.931 3 -1 4 -6 1129.28 366.753 2 -1 4 -7 18689.0 610.774 3 -1 4 -7 18434.7 1383.56 2 1 -4 7 18869.5 668.105 3 1 -4 8 22593.5 1168.23 2 1 -4 8 23831.7 776.118 3 -1 4 -8 21101.2 1552.87 2 1 -4 9 7530.62 690.745 2 1 -4 9 7701.72 453.170 3 1 -4 9 7103.29 417.138 1 -1 4 -9 7294.68 1030.12 2 1 -4 10 2340.41 257.668 3 1 -4 10 2346.95 244.375 1 -1 4 -11 155.796 531.786 2 1 -4 11 656.853 162.071 3 1 -4 11 627.600 136.575 1 1 -4 12 9567.13 520.528 3 -1 4 -12 8687.34 1166.20 2 -1 4 -13 2747.66 819.622 2 -1 4 -14 9687.70 1377.49 2 -1 3 15 605.325 308.016 3 1 -3 -14 5280.49 748.341 2 -1 3 14 4434.05 633.694 3 1 -3 -13 8008.56 902.793 2 1 -3 -12 490.088 323.456 2 1 -3 -12 1252.08 415.123 1 1 -3 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57783.3 1720.35 2 -2 5 -4 4824.29 667.781 2 2 -5 4 5869.53 347.413 1 -2 5 -4 5442.01 319.597 3 -2 5 -5 9993.34 401.964 3 2 -5 5 11050.3 452.441 1 -2 5 -5 10442.6 1020.39 2 2 -5 6 23476.4 665.505 1 -2 5 -6 22078.7 1509.07 2 -2 5 -6 23839.9 596.790 3 -2 5 -7 4223.21 223.213 3 -2 5 -7 3721.41 703.942 2 2 -5 7 4115.28 518.628 2 2 -5 7 4137.93 264.132 1 2 -5 8 22121.6 1151.14 2 -2 5 -8 20508.0 1593.82 2 2 -5 8 20497.0 572.363 1 2 -5 9 11486.6 434.191 1 -2 5 -9 11253.0 1208.34 2 2 -5 10 482.081 99.9957 1 -2 5 -10 755.001 538.648 2 2 -5 11 7277.24 282.667 1 -2 5 -11 9455.56 1245.62 2 -2 5 -12 9733.47 1296.89 2 -2 5 -13 10784.2 1435.78 2 -2 5 -14 4746.32 1054.76 2 -2 4 15 8883.92 917.955 3 -2 4 14 9218.53 938.963 3 2 -4 -13 15065.7 1132.53 2 2 -4 -12 186.865 353.799 1 2 -4 -12 321.333 285.508 2 2 -4 -11 11291.2 880.125 2 2 -4 -11 10285.1 965.042 1 2 -4 -10 1150.64 304.210 2 2 -4 -10 1643.99 442.439 1 2 -4 -9 321.791 214.320 2 2 -4 -9 900.269 379.477 1 -2 4 9 580.910 199.359 1 2 -4 -8 14327.5 974.702 1 -2 4 8 16373.5 754.056 1 2 -4 -8 15977.2 773.025 2 2 -4 -7 2187.22 278.688 2 -2 4 7 1972.95 269.640 1 2 -4 -6 80706.2 1539.94 2 -2 4 6 81515.2 1764.67 1 2 -4 -5 229392. 2995.52 2 2 -4 -5 219525. 3889.12 1 2 -4 -4 155274. 2927.76 1 2 -4 -3 220130. 3557.41 1 2 -4 -2 46987.5 1282.60 1 2 -4 -2 47038.2 1062.44 2 2 -4 -1 2173.01 259.517 1 2 -4 -1 2642.29 269.404 2 2 -4 0 756264. 8930.12 1 2 -4 0 762695. 9086.74 2 -2 4 0 765741. 9647.67 2 2 -4 1 57843.9 1206.60 1 -2 4 -1 58967.9 1135.11 1 -2 4 -1 58510.9 1742.14 2 2 -4 1 59868.5 1468.72 2 2 -4 2 151993. 2735.02 2 2 -4 2 152913. 2207.99 1 -2 4 -2 150717. 3202.18 2 -2 4 -2 151355. 2118.88 1 2 -4 3 143410. 2050.01 1 -2 4 -3 145751. 2032.19 3 -2 4 -3 144913. 3276.78 2 2 -4 4 156931. 2099.43 1 -2 4 -4 151777. 2026.05 3 -2 4 -4 155210. 3570.53 2 -2 4 -5 34237.5 616.763 3 2 -4 5 37490.9 722.660 1 -2 4 -5 36730.4 1688.56 2 -2 4 -6 342.612 329.806 2 2 -4 6 413.544 83.4003 1 2 -4 7 38996.8 771.560 1 -2 4 -7 36902.7 1904.60 2 2 -4 8 12486.7 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'No special instructions were received'