#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 10 _journal_issue 3 _journal_year 2019 _journal_page_first 201 _journal_page_last 208 #=============================================================================== data_shelx _publ_section_keywords ; crystal structure, cupper, Schiff base ; #Added by publCIF _publ_section_related_literature ; ; _publ_contact_author_name ; 'Mohamed Gaye' ; _publ_contact_author_address ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar S\'en\'egal ; _publ_contact_author_phone '00221338247804' _publ_contact_author_fax '00221338246318' _publ_contact_author_email 'mlgayeastou@yahoo.fr' _publ_requested_journal 'Acta Cryst. E' _publ_contact_letter ; ; _publ_requested_category EO _publ_section_title ; Title (type here to add) ; loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'Pokpa, Haba' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . . 'Adama, Sy' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . . 'Farba Bouyagui, Tamboura' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . . 'Mamour, Sarr' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . . 'Ibrahima Elhadji, Thiam' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . . 'Mohamed, Gaye' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; . ; mlgayeastou@yahoo.fr ; 'Aliou Hamady, Barry' ; D\'epartement de Chimie Facult\'e des Sciences Universit\'e de Nouakchott Nouakchott, Mauritanie ; . . 'Pascal, Retailleau' ; Institut de Chimie des Substances Naturelles, CNRS UPR 2301, Universit\'e Paris-Sud, Universit\'e Paris-Saclay., 1, av. de la Terrasse, 91198 Gif-sur-Yvette, France ; . . _publ_section_abstract ; (type here to add) ; _publ_section_references ; Bruker (2016). APEX3, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Farrugia, J. L. (2012). J. Appl. Cryst. 45, 849-854. Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8. Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8. ; _publ_section_figure_captions ; Fig. 1. An ORTEP view of the title compound, showing the atom-numbering scheme and intramolecular H bonds contacts. Displacement ellipsoids are plotted at the 50% probability level. Fig. 2.Molecular representation of the title compound, showing the intermolecular H bonds contacts. ; _publ_section_acknowledgements ; The authors are grateful to the Sonatel Foundation for financial support. ; _audit_update_record ; 2018-02-07 # Formatted by publCIF ; _publcif_datablock.id '{289c58f7-101e-443d-b2ff-5cad87d27cb5}' # publcif _publ_body_element loop start loop_ _publ_body_element _publ_body_title _publ_body_contents section ; Chemical context ; ; ; section ; Structural commentary ; ; Figure 1 shows the structure of the complex. The asymmetric unit contains a ...... ; section ; Supramolecular features ; ; In the crystal,....... ; section ; Database survey ; ; ; section ; Synthesis and crystallization ; ; A mixture of ...... ; section ; Refinement ; ; Crystal data, data collection and structure refinement details are summarized in Table 1. H atoms of =CH, CH~2~ and CH~3~ groups were geometrically optimized and refined as riding model by AFIX instructions with U~iso~(H) = 1.2U~eq~(C)(1.5 for CH~3~ and NH). H atoms of NH groups were generated from difference fourier map and refined using DFIX instructions. High thermal motion for S atom of one of the thiocyanate group was noted, indicating some disorder in their positions. This S atom was distributed over two sites.The occupancy factor refines close to 60:40%. ; # publcif _publ_body_element loop end _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H16 Cu N6 S2' _chemical_formula_sum 'C11 H16 Cu N6 S2' _chemical_formula_weight 359.96 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2578(7) _cell_length_b 7.4334(2) _cell_length_c 16.6237(5) _cell_angle_alpha 90 _cell_angle_beta 99.089(3) _cell_angle_gamma 90 _cell_volume 3203.95(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5990 _cell_measurement_theta_min 2.4120 _cell_measurement_theta_max 28.6423 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.492 _exptl_crystal_F_000 1480 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_absorpt_coefficient_mu 1.623 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 19919 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.615 _diffrn_reflns_theta_max 29.735 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.905 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.905 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 4128 _reflns_number_gt 3616 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_reduction 'SAINT (Bruker, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 2012)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2015b)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+3.2432P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4128 _refine_ls_number_parameters 187 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.38124(2) 0.46733(3) 0.43752(2) 0.03209(10) Uani 1 1 d . . . . . S1 S 0.45042(4) 0.04276(15) 0.63427(7) 0.0908(3) Uani 1 1 d . . . . . N1 N 0.34354(7) 0.5960(2) 0.51907(10) 0.0380(4) Uani 1 1 d . . . . . C1 C 0.33639(8) 0.7766(3) 0.49898(13) 0.0357(4) Uani 1 1 d . . . . . S2 S 0.25338(3) 0.09667(10) 0.26800(4) 0.0604(2) Uani 1 1 d . . . . . N2 N 0.30228(8) 0.7277(3) 0.60699(12) 0.0459(4) Uani 1 1 d D . . . . C2 C 0.31099(8) 0.8606(3) 0.55426(14) 0.0399(4) Uani 1 1 d . . . . . N3 N 0.37757(7) 0.7132(2) 0.39103(11) 0.0391(4) Uani 1 1 d . . . . . C3 C 0.32205(10) 0.5719(3) 0.58404(14) 0.0459(5) Uani 1 1 d . . . . . H3 H 0.320599 0.462494 0.610719 0.055 Uiso 1 1 calc R U . . . C4 C 0.35595(8) 0.8348(3) 0.42765(14) 0.0409(4) Uani 1 1 d . . . . . H4 H 0.353054 0.953186 0.409370 0.049 Uiso 1 1 calc R U . . . N4 N 0.42815(7) 0.4300(3) 0.34831(12) 0.0405(4) Uani 1 1 d . . . . . C5 C 0.40013(12) 0.7431(4) 0.31678(16) 0.0546(6) Uani 1 1 d . . . . . H5A H 0.433121 0.803782 0.329461 0.066 Uiso 1 1 calc R U . . . H5AB H 0.377331 0.815615 0.278102 0.066 Uiso 1 1 calc R U . . . N5 N 0.41283(8) 0.2776(3) 0.51019(13) 0.0501(5) Uani 1 1 d . . . . . N6 N 0.31799(7) 0.3213(3) 0.37218(12) 0.0448(4) Uani 1 1 d . . . . . C6 C 0.40683(11) 0.5575(4) 0.28243(15) 0.0518(6) Uani 1 1 d . . . . . H6A H 0.373757 0.513540 0.255242 0.062 Uiso 1 1 calc R U . . . H6AB H 0.429974 0.564254 0.242462 0.062 Uiso 1 1 calc R U . . . C7 C 0.42701(11) 0.2451(4) 0.3150(2) 0.0598(7) Uani 1 1 d . . . . . H7A H 0.450105 0.237150 0.275773 0.090 Uiso 1 1 calc R U . . . H7AB H 0.392625 0.216647 0.289207 0.090 Uiso 1 1 calc R U . . . H7AC H 0.437572 0.161473 0.358471 0.090 Uiso 1 1 calc R U . . . C10 C 0.42828(8) 0.1789(3) 0.56082(15) 0.0448(5) Uani 1 1 d . . . . . C8 C 0.48171(10) 0.4748(5) 0.3835(2) 0.0632(8) Uani 1 1 d . . . . . H8A H 0.502951 0.471452 0.341520 0.095 Uiso 1 1 calc R U . . . H8AB H 0.494263 0.388932 0.425072 0.095 Uiso 1 1 calc R U . . . H8AC H 0.482814 0.593133 0.406825 0.095 Uiso 1 1 calc R U . . . C9 C 0.29537(12) 1.0505(4) 0.5620(2) 0.0578(7) Uani 1 1 d . . . . . H9A H 0.311908 1.097754 0.613293 0.087 Uiso 1 1 calc R U . . . H9AB H 0.258622 1.056879 0.559356 0.087 Uiso 1 1 calc R U . . . H9AC H 0.305440 1.119910 0.518441 0.087 Uiso 1 1 calc R U . . . C11 C 0.29096(8) 0.2287(3) 0.32944(12) 0.0349(4) Uani 1 1 d . . . . . HN2 H 0.2880(9) 0.741(4) 0.6470(12) 0.042 Uiso 1 1 d D 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 Cu1 0.03810(15) 0.02905(15) 0.03026(14) 0.00065(8) 0.00894(10) 0.00118(8) S1 0.0903(6) 0.0877(7) 0.0880(7) 0.0496(5) -0.0055(5) 0.0123(5) N1 0.0507(9) 0.0345(8) 0.0302(8) -0.0016(7) 0.0113(7) -0.0007(7) C1 0.0394(9) 0.0334(9) 0.0365(10) -0.0021(8) 0.0130(8) 0.0005(8) S2 0.0880(5) 0.0547(4) 0.0422(3) -0.0108(3) 0.0215(3) -0.0372(4) N2 0.0516(10) 0.0569(12) 0.0333(9) -0.0081(9) 0.0191(8) -0.0022(9) C2 0.0363(9) 0.0437(11) 0.0414(11) -0.0079(9) 0.0111(8) 0.0009(8) N3 0.0524(10) 0.0345(8) 0.0346(9) 0.0039(7) 0.0197(7) 0.0044(7) C3 0.0618(13) 0.0450(12) 0.0339(11) 0.0013(9) 0.0172(10) -0.0040(10) C4 0.0502(11) 0.0310(10) 0.0450(11) 0.0048(9) 0.0184(9) 0.0047(8) N4 0.0411(9) 0.0405(9) 0.0426(10) -0.0050(8) 0.0152(7) 0.0014(7) C5 0.0778(17) 0.0471(13) 0.0473(13) 0.0108(11) 0.0356(12) 0.0076(12) N5 0.0494(10) 0.0482(11) 0.0515(11) 0.0121(9) 0.0041(9) 0.0067(9) N6 0.0397(9) 0.0482(11) 0.0460(10) -0.0059(9) 0.0047(8) -0.0008(8) C6 0.0674(15) 0.0560(14) 0.0374(12) 0.0009(10) 0.0247(11) 0.0074(12) C7 0.0644(15) 0.0498(14) 0.0718(18) -0.0184(13) 0.0314(13) 0.0044(12) C10 0.0397(10) 0.0436(12) 0.0502(13) 0.0072(10) 0.0042(9) 0.0031(9) C8 0.0413(12) 0.078(2) 0.0729(19) -0.0048(15) 0.0173(12) -0.0087(12) C9 0.0619(15) 0.0496(14) 0.0683(17) -0.0094(12) 0.0297(13) 0.0118(11) C11 0.0418(10) 0.0321(9) 0.0337(10) 0.0029(8) 0.0153(8) 0.0021(8) _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 N5 1.954(2) . y Cu1 N3 1.9809(18) . y Cu1 N1 2.0389(18) . y Cu1 N4 2.0905(18) . y Cu1 N6 2.1322(19) . y S1 C10 1.621(2) . y N1 C3 1.307(3) . ? N1 C1 1.389(3) . ? C1 C2 1.369(3) . ? C1 C4 1.432(3) . ? S2 C11 1.631(2) . y N2 C3 1.349(3) . ? N2 C2 1.364(3) . ? N2 HN2 0.820(17) . ? C2 C9 1.481(3) . ? N3 C4 1.273(3) . ? N3 C5 1.468(3) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? N4 C8 1.473(3) . ? N4 C7 1.481(3) . ? N4 C6 1.489(3) . ? C5 C6 1.514(4) . ? C5 H5A 0.9700 . ? C5 H5AB 0.9700 . ? N5 C10 1.142(3) . y N6 C11 1.150(3) . y C6 H6A 0.9700 . ? C6 H6AB 0.9700 . ? C7 H7A 0.9600 . ? C7 H7AB 0.9600 . ? C7 H7AC 0.9600 . ? C8 H8A 0.9600 . ? C8 H8AB 0.9600 . ? C8 H8AC 0.9600 . ? C9 H9A 0.9600 . ? C9 H9AB 0.9600 . ? C9 H9AC 0.9600 . ? 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 N5 Cu1 N3 153.72(9) . . y N5 Cu1 N1 97.51(8) . . y N3 Cu1 N1 80.08(7) . . y N5 Cu1 N4 95.89(9) . . y N3 Cu1 N4 80.99(7) . . y N1 Cu1 N4 159.44(7) . . y N5 Cu1 N6 99.67(9) . . y N3 Cu1 N6 106.56(8) . . y N1 Cu1 N6 99.01(7) . . y N4 Cu1 N6 94.01(8) . . y C3 N1 C1 105.76(18) . . ? C3 N1 Cu1 143.43(17) . . ? C1 N1 Cu1 110.78(13) . . ? C2 C1 N1 109.95(19) . . ? C2 C1 C4 134.0(2) . . ? N1 C1 C4 116.03(17) . . ? C3 N2 C2 109.22(18) . . ? C3 N2 HN2 125.1(19) . . ? C2 N2 HN2 125.6(19) . . ? N2 C2 C1 104.48(19) . . ? N2 C2 C9 123.9(2) . . ? C1 C2 C9 131.6(2) . . ? C4 N3 C5 124.4(2) . . ? C4 N3 Cu1 117.82(14) . . ? C5 N3 Cu1 117.80(15) . . ? N1 C3 N2 110.6(2) . . ? N1 C3 H3 124.7 . . ? N2 C3 H3 124.7 . . ? N3 C4 C1 115.28(19) . . ? N3 C4 H4 122.4 . . ? C1 C4 H4 122.4 . . ? C8 N4 C7 108.6(2) . . ? C8 N4 C6 111.9(2) . . ? C7 N4 C6 109.4(2) . . ? C8 N4 Cu1 108.71(17) . . ? C7 N4 Cu1 114.15(15) . . ? C6 N4 Cu1 104.02(13) . . ? N3 C5 C6 105.41(19) . . ? N3 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? N3 C5 H5AB 110.7 . . ? C6 C5 H5AB 110.7 . . ? H5A C5 H5AB 108.8 . . ? C10 N5 Cu1 170.4(2) . . ? C11 N6 Cu1 166.98(17) . . ? N4 C6 C5 110.8(2) . . ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N4 C6 H6AB 109.5 . . ? C5 C6 H6AB 109.5 . . ? H6A C6 H6AB 108.1 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7AB 109.5 . . ? H7A C7 H7AB 109.5 . . ? N4 C7 H7AC 109.5 . . ? H7A C7 H7AC 109.5 . . ? H7AB C7 H7AC 109.5 . . ? N5 C10 S1 178.6(3) . . y N4 C8 H8A 109.5 . . ? N4 C8 H8AB 109.5 . . ? H8A C8 H8AB 109.5 . . ? N4 C8 H8AC 109.5 . . ? H8A C8 H8AC 109.5 . . ? H8AB C8 H8AC 109.5 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9AB 109.5 . . ? H9A C9 H9AB 109.5 . . ? C2 C9 H9AC 109.5 . . ? H9A C9 H9AC 109.5 . . ? H9AB C9 H9AC 109.5 . . ? N6 C11 S2 179.07(19) . . y 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 C3 N1 C1 C2 1.1(2) . . . . ? Cu1 N1 C1 C2 179.92(14) . . . . ? C3 N1 C1 C4 -178.6(2) . . . . ? Cu1 N1 C1 C4 0.2(2) . . . . ? C3 N2 C2 C1 0.4(3) . . . . ? C3 N2 C2 C9 -178.7(2) . . . . ? N1 C1 C2 N2 -0.9(2) . . . . ? C4 C1 C2 N2 178.8(2) . . . . ? N1 C1 C2 C9 178.1(2) . . . . ? C4 C1 C2 C9 -2.2(4) . . . . ? C1 N1 C3 N2 -0.9(3) . . . . ? Cu1 N1 C3 N2 -178.98(19) . . . . ? C2 N2 C3 N1 0.3(3) . . . . ? C5 N3 C4 C1 179.8(2) . . . . ? Cu1 N3 C4 C1 -0.4(3) . . . . ? C2 C1 C4 N3 -179.6(2) . . . . ? N1 C1 C4 N3 0.1(3) . . . . ? C4 N3 C5 C6 -164.0(2) . . . . ? Cu1 N3 C5 C6 16.2(3) . . . . ? C8 N4 C6 C5 -67.8(3) . . . . ? C7 N4 C6 C5 171.7(2) . . . . ? Cu1 N4 C6 C5 49.3(2) . . . . ? N3 C5 C6 N4 -43.4(3) . . . . ? 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 N2 HN2 S2 0.820(17) 2.629(19) 3.406(2) 159(2) 6_566 C7 H7AB N6 0.96 2.68 3.206(3) 114.7 . C9 H9AB N6 0.96 2.62 3.463(3) 146.2 7_566 _refine_diff_density_max 1.374 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.085 _shelx_res_file ; TITL exp_1_a.res in C2/c shelx.res created by SHELXL-2014/7 at 09:03:03 on 08-Feb-2019 CELL 0.71073 26.2578 7.4334 16.6237 90.000 99.089 90.000 ZERR 8.00 0.0007 0.0002 0.0005 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H CU N S UNIT 88 128 8 48 16 MERG 2 OMIT 5 1 4 OMIT -4 0 4 OMIT -5 3 2 OMIT -7 1 1 OMIT -3 1 2 OMIT 3 1 2 OMIT -3 1 1 OMIT -3 1 3 DFIX 0.87 N2 HN2 EQIV $1 x, -y+1, z+1/2 HTAB N2 S2_$1 HTAB C7 N6 EQIV $2 -x+1/2, -y+3/2, -z+1 HTAB C9 N6_$2 FMAP 2 PLAN 20 ACTA HTAB BOND $H CONF LIST 4 L.S. 10 WGHT 0.055900 3.243200 FVAR 0.46949 CU1 3 0.381241 0.467333 0.437517 11.00000 0.03810 0.02905 = 0.03026 0.00065 0.00894 0.00118 S1 5 0.450420 0.042761 0.634266 11.00000 0.09033 0.08770 = 0.08800 0.04956 -0.00549 0.01226 N1 4 0.343537 0.596012 0.519072 11.00000 0.05074 0.03448 = 0.03023 -0.00161 0.01126 -0.00073 C1 1 0.336389 0.776600 0.498977 11.00000 0.03940 0.03340 = 0.03647 -0.00213 0.01303 0.00050 S2 5 0.253382 0.096673 0.267999 11.00000 0.08798 0.05467 = 0.04220 -0.01082 0.02145 -0.03717 N2 4 0.302284 0.727738 0.606989 11.00000 0.05164 0.05686 = 0.03333 -0.00810 0.01907 -0.00219 C2 1 0.310992 0.860623 0.554261 11.00000 0.03632 0.04366 = 0.04138 -0.00791 0.01107 0.00087 N3 4 0.377573 0.713232 0.391030 11.00000 0.05241 0.03454 = 0.03458 0.00385 0.01970 0.00435 C3 1 0.322052 0.571897 0.584036 11.00000 0.06181 0.04503 = 0.03394 0.00131 0.01721 -0.00403 AFIX 43 H3 2 0.320599 0.462494 0.610719 11.00000 -1.20000 AFIX 0 C4 1 0.355948 0.834828 0.427652 11.00000 0.05016 0.03099 = 0.04502 0.00485 0.01836 0.00469 AFIX 43 H4 2 0.353054 0.953186 0.409370 11.00000 -1.20000 AFIX 0 N4 4 0.428148 0.430022 0.348309 11.00000 0.04108 0.04052 = 0.04258 -0.00503 0.01520 0.00135 C5 1 0.400126 0.743079 0.316785 11.00000 0.07785 0.04706 = 0.04726 0.01077 0.03557 0.00755 AFIX 23 H5A 2 0.433121 0.803782 0.329461 11.00000 -1.20000 H5AB 2 0.377331 0.815615 0.278102 11.00000 -1.20000 AFIX 0 N5 4 0.412831 0.277639 0.510190 11.00000 0.04945 0.04822 = 0.05149 0.01210 0.00406 0.00670 N6 4 0.317993 0.321315 0.372176 11.00000 0.03969 0.04817 = 0.04595 -0.00589 0.00466 -0.00076 C6 1 0.406828 0.557452 0.282429 11.00000 0.06738 0.05595 = 0.03736 0.00094 0.02467 0.00738 AFIX 23 H6A 2 0.373757 0.513540 0.255242 11.00000 -1.20000 H6AB 2 0.429974 0.564254 0.242462 11.00000 -1.20000 AFIX 0 C7 1 0.427013 0.245064 0.315013 11.00000 0.06438 0.04977 = 0.07184 -0.01841 0.03140 0.00438 AFIX 137 H7A 2 0.450105 0.237150 0.275773 11.00000 -1.50000 H7AB 2 0.392625 0.216647 0.289207 11.00000 -1.50000 H7AC 2 0.437572 0.161473 0.358471 11.00000 -1.50000 AFIX 0 C10 1 0.428278 0.178896 0.560823 11.00000 0.03968 0.04358 = 0.05023 0.00719 0.00415 0.00313 C8 1 0.481710 0.474784 0.383497 11.00000 0.04126 0.07822 = 0.07289 -0.00476 0.01732 -0.00870 AFIX 137 H8A 2 0.502951 0.471452 0.341520 11.00000 -1.50000 H8AB 2 0.494263 0.388932 0.425072 11.00000 -1.50000 H8AC 2 0.482814 0.593133 0.406825 11.00000 -1.50000 AFIX 0 C9 1 0.295366 1.050493 0.562020 11.00000 0.06194 0.04958 = 0.06826 -0.00943 0.02968 0.01177 AFIX 137 H9A 2 0.311908 1.097754 0.613293 11.00000 -1.50000 H9AB 2 0.258622 1.056879 0.559356 11.00000 -1.50000 H9AC 2 0.305440 1.119910 0.518441 11.00000 -1.50000 AFIX 0 C11 1 0.290960 0.228664 0.329443 11.00000 0.04181 0.03212 = 0.03366 0.00288 0.01526 0.00209 HN2 2 0.287991 0.740569 0.647028 11.00000 -1.20000 HKLF 4 REM exp_1_a.res in C2/c REM R1 = 0.0370 for 3616 Fo > 4sig(Fo) and 0.0435 for all 4128 data REM 187 parameters refined using 1 restraints END WGHT 0.0559 3.2432 REM Instructions for potential hydrogen bonds HTAB C7 N6 HTAB C9 N6_$2 HTAB N2 S2_$1 REM Highest difference peak 1.374, deepest hole -1.070, 1-sigma level 0.085 Q1 1 0.4591 -0.0116 0.5875 11.00000 0.05 1.37 Q2 1 0.2826 0.0582 0.2783 11.00000 0.05 0.40 Q3 1 0.4824 0.5420 0.4407 11.00000 0.05 0.26 Q4 1 0.4213 0.4787 0.3184 11.00000 0.05 0.26 Q5 1 0.4503 0.4472 0.3588 11.00000 0.05 0.24 Q6 1 0.3496 0.7887 0.2498 11.00000 0.05 0.24 Q7 1 0.3158 0.8115 0.5184 11.00000 0.05 0.23 Q8 1 0.2775 1.1079 0.4887 11.00000 0.05 0.22 Q9 1 0.4689 0.6963 0.3952 11.00000 0.05 0.22 Q10 1 0.3621 0.7739 0.3958 11.00000 0.05 0.22 Q11 1 0.3621 0.8960 0.2121 11.00000 0.05 0.22 Q12 1 0.3196 0.8569 0.2513 11.00000 0.05 0.21 Q13 1 0.4017 0.9586 0.2220 11.00000 0.05 0.21 Q14 1 0.3281 0.8606 0.2129 11.00000 0.05 0.21 Q15 1 0.5018 0.5639 0.4832 11.00000 0.05 0.21 Q16 1 0.2981 0.9265 0.5404 11.00000 0.05 0.21 Q17 1 0.3519 0.9043 0.2603 11.00000 0.05 0.21 Q18 1 0.5174 0.3774 0.5079 11.00000 0.05 0.21 Q19 1 0.4249 0.4665 0.3750 11.00000 0.05 0.20 Q20 1 0.4271 0.3441 0.3441 11.00000 0.05 0.20 ; _shelx_res_checksum 74570 _shelx_hkl_file ; 0 0 -3-0.12583 0.40753 3 0 0 -4 2197.28 99.4864 3 0 0 5 1.14874 1.39176 3 0 0 6 5574.65 251.365 3 0 0 7-0.92570 3.33968 1 0 0 7 2.42950 1.91397 3 0 0 8 570.970 27.3204 3 0 0 8 584.971 28.7784 1 0 0 -8 601.194 28.3413 2 0 0 -9-0.45288 3.76353 2 0 0 9-0.30433 4.96289 1 0 0 9 1.21212 2.59492 3 0 0 -10 1654.94 77.5518 2 0 0 10 1780.45 78.6843 1 0 0 10 1642.34 76.5918 3 0 0 -11 1.60657 4.92349 2 0 0 11 2.44075 3.35923 3 0 0 11 2.59563 5.69561 1 0 0 -12 40.5419 6.24141 2 0 0 12 24.5560 4.53929 3 0 0 12 29.1746 6.85895 1 0 0 13 1.72377 6.95415 1 0 0 -13-0.62163 6.18322 2 0 0 13 1.56344 3.97641 3 0 0 14 1389.78 66.0356 3 0 0 14 1421.88 68.5493 1 0 0 -14 1478.68 67.3522 2 0 0 -15-7.98287 6.95406 2 0 0 15-2.93161 8.30575 1 0 0 15-0.22813 5.19607 3 0 0 16 1518.80 74.4381 1 0 0 -16 1537.34 73.2186 2 0 0 16 1561.91 71.8708 3 0 0 -17-1.15714 8.06600 2 0 0 17-4.94975 9.28679 1 0 0 17-7.83717 5.98043 3 0 0 18 850.794 39.5925 3 0 0 18 780.275 42.4685 1 0 0 -18 782.640 40.7870 2 0 0 -19 0.42622 7.19458 2 0 0 19-4.31049 10.1164 1 0 0 19 3.80371 6.90676 3 0 0 20 32.6338 10.5990 1 0 0 -20 37.1233 9.78469 2 0 0 -21 10.8185 8.97916 2 0 0 21-1.33036 11.2002 1 0 0 -22 62.4783 10.9924 2 0 2 0 3868.79 161.285 2 0 -2 0 3285.55 161.249 2 0 -2 -1 225.042 11.0905 1 0 -2 1 222.610 11.0922 2 0 -2 -1 206.823 11.1132 2 0 2 -1 245.337 11.1276 2 0 2 1 245.671 11.3398 2 0 -2 2 999.591 47.7523 2 0 2 -2 1068.51 47.6984 2 0 2 2 1069.94 48.0711 2 0 2 3 15286.5 732.741 2 0 2 -3 16866.6 732.222 2 0 2 -4 164.502 8.63755 2 0 -2 -4 176.840 8.75294 3 0 -2 -5 186.579 9.39424 3 0 -2 -6 7444.36 335.488 3 0 -2 -7 757.012 35.0797 3 0 -2 7 670.515 37.0761 1 0 2 7 747.648 35.2107 3 0 2 8 1729.12 81.8653 3 0 2 8 1811.06 81.8425 1 0 -2 -8 1751.14 81.8595 3 0 -2 8 1876.06 84.5716 1 0 -2 -8 1946.96 83.1799 2 0 -2 -9 25.4061 5.18937 2 0 -2 9 20.9128 6.50357 1 0 2 9 23.9976 3.45439 3 0 2 9 18.4955 3.44077 1 0 -2 -9 27.9043 2.53946 3 0 -2 10 4317.45 203.449 3 0 2 10 4491.68 202.606 1 0 -2 -10 4693.72 203.687 2 0 -2 -10 4467.94 202.288 3 0 2 10 4401.99 202.210 3 0 -2 10 4550.81 205.299 1 0 -2 -11 490.078 24.2148 2 0 -2 -11 445.876 22.2797 3 0 -2 11 476.793 24.0718 3 0 2 11 456.489 22.3479 3 0 -2 11 462.350 25.8987 1 0 2 11 457.370 23.1155 1 0 2 12 294.548 16.2744 1 0 -2 12 300.589 17.0815 3 0 -2 -12 323.854 17.4579 2 0 2 12 304.446 15.3348 3 0 -2 -12 276.639 15.1199 3 0 -2 12 308.660 19.4613 1 0 -2 -13 415.723 22.1609 3 0 2 13 446.734 22.1745 3 0 -2 13 470.382 24.0689 3 0 -2 -13 504.487 24.4025 2 0 -2 13 458.062 26.3753 1 0 2 13 455.995 23.3416 1 0 -2 -14 1729.00 77.8904 2 0 2 14 1591.69 75.9065 3 0 -2 14 1513.70 79.5724 1 0 2 14 1681.95 77.3051 1 0 -2 14 1730.43 77.5365 3 0 -2 -15 51.2152 8.87559 2 0 2 15 36.3842 7.65837 1 0 -2 15 42.4634 10.4063 1 0 -2 15 30.6449 7.53788 3 0 2 15 38.8268 5.78181 3 0 -2 16 194.162 13.1757 3 0 -2 -16 185.744 13.5225 2 0 2 -16 166.348 13.0544 2 0 2 16 165.469 10.7876 3 0 2 16 183.120 12.9375 1 0 -2 16 144.093 15.2070 1 0 -2 17 386.838 20.3934 3 0 2 -17 335.778 20.1628 2 0 -2 -17 333.295 20.8463 2 0 -2 17 307.830 22.3861 1 0 2 17 349.076 18.4633 3 0 2 17 352.635 20.4547 1 0 2 -18 28.8603 8.81436 2 0 -2 18 17.0676 9.81871 1 0 -2 18 17.5153 7.55911 3 0 2 18 27.5490 8.80742 1 0 2 18 25.4174 6.41783 3 0 -2 -18 26.4436 10.1901 2 0 -2 -19-3.22914 9.94427 2 0 2 -19 0.42597 8.55951 2 0 -2 19 5.89485 8.14085 3 0 -2 19-0.73982 11.5519 1 0 2 19 11.4868 8.84426 1 0 2 -20 18.8051 9.40654 2 0 -2 20 12.4715 12.3293 1 0 -2 20 21.6703 9.15215 3 0 -2 -20 9.18193 10.2003 2 0 -2 -21 65.1976 11.9511 2 0 2 -21 84.5090 11.0016 2 0 -2 21 65.7021 13.5144 1 0 4 0 5288.56 240.053 2 0 -4 0 5352.90 240.865 1 0 -4 0 5289.04 240.406 2 0 -4 -1 580.183 27.3933 2 0 -4 1 589.136 27.2431 2 0 4 1 528.710 27.1150 2 0 4 -1 560.726 26.9938 2 0 -4 1 555.564 28.0057 1 0 -4 -1 570.377 27.3791 1 0 -4 -2 1247.38 56.8244 2 0 4 2 1256.98 56.7434 2 0 -4 2 1187.73 57.7653 1 0 -4 -2 1252.62 56.3492 1 0 -4 2 1170.57 56.4458 2 0 4 -2 1195.58 56.1976 2 0 -4 -3 6790.83 317.482 2 0 4 -3 7055.17 316.891 2 0 4 3 7387.03 317.591 2 0 -4 3 6913.88 317.223 2 0 -4 -3 7054.81 316.533 1 0 -4 3 6844.48 318.781 1 0 -4 -4 1439.64 63.1618 1 0 4 -4 1417.70 64.2740 2 0 -4 4 1421.30 64.6932 2 0 -4 -4 1341.31 64.9342 2 0 -4 -4 1341.95 63.2540 1 0 -4 4 1324.78 66.3001 1 0 4 4 1467.99 65.2540 2 0 4 5 51.1821 5.90226 2 0 -4 -5 29.3076 3.80729 3 0 -4 -5 38.3339 3.87663 2 0 4 -5 43.4338 4.25579 2 0 -4 5 29.6621 4.61533 1 0 -4 6 2.32356 3.38977 1 0 4 -6 3.54894 3.39579 2 0 -4 -6 6.58906 2.62172 3 0 -4 -6 3.25807 2.45928 2 0 4 6 7.72440 5.17634 2 0 -4 -7 1113.70 51.5924 3 0 4 -7 1062.06 50.8515 2 0 4 7 1209.62 52.8108 2 0 -4 7 1018.12 53.5003 1 0 -4 -8 767.467 34.5037 3 0 -4 8 667.329 36.7732 1 0 4 -8 696.540 34.0357 2 0 -4 -9 6.91917 2.40444 3 0 4 -9 13.7581 4.41567 2 0 -4 -10 77.5514 5.57830 3 0 4 -10 71.9701 6.50689 2 0 -4 -11 703.170 36.7375 2 0 -4 -11 709.639 34.8457 3 0 4 -11 778.484 35.5034 2 0 -4 -12 3.23698 2.38371 3 0 -4 -12 3.15497 7.51715 2 0 4 -12-6.52040 5.77126 2 0 -4 13 194.894 17.0159 1 0 -4 -13 236.850 12.3130 3 0 4 -13 210.236 13.6321 2 0 -4 -13 248.595 15.9583 2 0 -4 14 7.40851 9.81146 1 0 -4 14 11.0371 9.01165 3 0 -4 -14 32.6474 8.68133 2 0 -4 -14 27.1903 3.40728 3 0 4 -14 19.1302 6.09970 2 0 4 -15 5.54838 6.18505 2 0 -4 15 14.6957 10.7164 1 0 -4 -15 4.99384 8.75206 2 0 -4 -15 13.4808 3.03314 3 0 -4 15 7.92668 9.16644 3 0 -4 -16 532.339 26.3271 3 0 -4 -16 559.609 29.6945 2 0 -4 16 494.625 31.9712 1 0 4 -16 497.805 27.2841 2 0 -4 16 598.845 30.7488 3 0 -4 17 167.201 15.1446 3 0 4 -17 142.609 11.1522 2 0 -4 -17 173.127 14.2172 2 0 -4 -17 152.105 9.51376 3 0 -4 17 142.995 17.2219 1 0 -4 18 239.789 17.3362 3 0 -4 18 186.006 19.7896 1 0 -4 -18 177.564 15.7771 2 0 -4 19 46.6698 11.9888 3 0 4 -19 20.6635 9.20432 2 0 -4 20 16.8527 11.1680 3 0 6 0 367.558 19.5120 2 0 -6 0 394.628 19.8134 2 0 -6 0 347.056 19.6279 1 0 -6 -1 928.896 40.6372 2 0 -6 1 832.817 40.0005 2 0 6 1 825.757 39.9833 2 0 -6 1 794.310 40.5960 1 0 6 -1 806.951 39.6228 2 0 -6 -1 785.739 39.8727 1 0 -6 2 747.968 37.2276 2 0 6 -2 766.813 37.0513 2 0 -6 2 805.036 38.7030 1 0 6 2 768.553 37.6326 2 0 -6 -2 742.906 36.8694 1 0 -6 -2 811.674 37.9312 2 0 -6 3 2221.07 102.138 2 0 -6 -3 2374.53 102.937 2 0 -6 -3 2214.49 101.262 1 0 -6 3 2155.95 103.762 1 0 6 -3 2181.07 101.649 2 0 6 3 2146.73 102.344 2 0 -6 4 256.906 14.7869 2 0 -6 4 255.253 16.4439 1 0 -6 -4 272.429 15.3529 2 0 -6 -4 265.286 13.2557 1 0 6 -4 260.275 14.7128 2 0 6 4 307.022 16.2463 2 0 6 -5 1152.14 54.6764 2 0 6 5 1199.54 56.0950 2 0 -6 -5 1176.11 55.9009 2 0 -6 5 1150.05 57.4548 1 0 6 6 497.261 25.9899 2 0 -6 -6 487.290 25.1941 2 0 6 -6 496.151 24.3285 2 0 -6 6 450.141 26.7962 1 0 -6 -6 478.637 25.2688 3 0 -6 7-1.25105 4.94678 1 0 6 7 4.08143 6.93747 2 0 -6 -7 2.15304 3.30306 3 0 6 -7 3.61724 5.24147 2 0 -6 -7 1.52642 3.22155 2 0 -6 -8 315.078 17.5284 2 0 6 -8 305.848 16.6918 2 0 6 8 312.285 18.7848 2 0 -6 -8 321.476 17.2336 3 0 -6 8 284.840 19.2664 1 0 6 -9-1.18002 5.42686 2 0 -6 -9 2.98720 3.12550 3 0 -6 9-2.09585 5.52451 1 0 -6 -9 0.83607 3.28504 2 0 6 9 7.74964 7.88702 2 0 -6 -10 108.637 7.80368 3 0 -6 -10 108.366 8.56669 2 0 -6 10 91.0351 10.0451 1 0 6 10 86.6377 11.3831 2 0 6 -10 107.547 8.67178 2 0 -6 11 924.473 53.2501 1 0 -6 -11 1031.11 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69.9053 1 4 2 -2 1553.69 69.2894 2 4 2 -2 1536.51 69.9296 1 -4 2 2 1552.70 69.3034 2 -4 -2 1 2008.12 95.8063 1 4 2 -1 2195.35 95.5999 2 4 -2 -1 2050.88 95.1978 1 4 2 -1 2131.33 95.8266 1 4 -2 -1 2092.53 95.1772 2 -4 2 1 2125.35 95.2289 2 -4 2 0 40.4975 2.65796 2 4 -2 0 36.5222 2.36588 2 4 2 0 38.4155 3.36126 1 -4 -2 0 38.1840 2.81768 1 -4 -2 -1 2099.02 94.9444 1 4 -2 1 2116.57 94.4997 2 4 2 1 2036.02 94.9863 1 -4 -2 -2 2382.90 106.405 1 4 2 2 2470.47 106.545 1 4 -2 2 2314.28 106.085 2 -4 -2 -2 2230.03 107.053 3 -4 -2 -3 137.817 7.35375 3 4 2 3 135.565 7.79302 3 -4 -2 -3 114.838 7.37745 2 -4 -2 -3 132.339 6.52442 1 4 2 4 2112.76 98.3628 3 4 2 4 2151.64 97.5079 1 -4 -2 -4 2252.78 98.3738 2 -4 -2 -4 2110.06 98.2447 3 -4 -2 -5 2975.53 140.533 3 -4 -2 -5 3404.61 140.865 2 4 2 5 3078.14 139.848 1 4 2 5 3143.29 140.768 3 4 -2 5 3070.01 141.307 3 4 2 5 2946.51 140.937 2 -4 -2 -6 102.705 6.30764 3 4 2 6 101.028 6.87769 3 4 2 6 112.897 6.93849 2 4 2 6 107.997 5.78299 1 4 -2 6 96.3341 7.57042 3 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2.25513 1 -11 -3 0 2.22777 4.16015 2 -11 -3 0 1.40493 2.23495 1 11 -3 0 7.28463 1.45917 2 11 -3 1 1779.67 84.8456 1 11 -3 1 1779.49 85.2653 3 -11 -3 -1 1794.43 84.8225 1 11 3 1 1784.92 85.0213 2 11 -3 1 1885.88 83.4042 2 11 3 1 1832.74 85.5015 1 -11 -3 -1 1931.94 85.1721 2 11 -3 2 1996.46 95.7206 3 -11 -3 -2 2014.08 94.9123 1 -11 -3 -2 2184.46 95.4819 2 11 3 2 2216.37 95.7102 1 11 -3 2 2001.08 95.2960 1 11 3 2 2042.99 95.4503 2 11 -3 3 996.263 49.1605 3 11 3 3 1089.55 48.9854 1 -11 -3 -3 1093.42 48.9482 2 11 3 3 1025.78 48.9055 2 11 3 3 1058.89 49.8729 3 11 -3 3 1003.94 48.8898 1 -11 -3 -3 1013.09 48.9764 3 -11 -3 -3 997.148 48.1458 1 11 -3 4 2340.45 114.839 3 -11 -3 -4 2683.99 114.673 2 -11 -3 -4 2422.51 113.721 1 11 3 4 2468.68 114.700 2 11 3 4 2566.35 115.444 3 -11 -3 -4 2408.91 114.611 3 11 3 4 2603.70 114.442 1 11 3 5 2738.56 122.264 1 -11 -3 -5 2742.25 121.886 1 -11 -3 -5 2718.76 122.452 2 11 3 5 2560.37 122.693 2 11 3 5 2681.63 123.316 3 -11 -3 -5 2537.56 122.670 3 -11 -3 -6 583.301 28.0728 2 11 3 6 548.550 28.1824 2 11 3 6 557.357 28.8514 3 -11 -3 -6 552.836 28.0853 3 11 3 6 565.002 27.6640 1 -11 -3 -7 212.761 13.0645 3 11 3 7 230.808 12.8517 1 -11 -3 -7 253.937 13.7332 2 11 3 7 230.850 13.4617 2 11 3 7 226.123 14.5693 3 11 3 8 241.314 14.4753 1 -11 -3 -8 281.461 15.3660 2 11 3 8 260.284 15.8602 3 11 3 8 264.433 15.1752 2 -11 -3 -8 266.650 14.9918 3 11 -3 8 283.420 16.2708 3 11 -3 9 137.423 11.0871 3 11 3 9 119.950 8.94569 1 -11 -3 -9 115.958 9.79446 2 11 3 9 121.693 10.3111 3 11 3 9 130.549 9.20596 2 -11 -3 -9 127.630 9.01978 3 11 3 10 824.593 42.6584 2 -11 -3 -10 817.058 41.9416 2 11 3 10 925.156 41.3337 1 11 3 10 856.028 42.7475 3 11 -3 10 908.531 43.2924 3 -11 -3 -10 852.000 42.3414 3 11 3 11 38.8036 5.83915 2 11 -3 11 50.7975 9.23124 3 11 3 11 41.9628 5.72211 1 -11 -3 -11 40.2392 7.00059 2 11 3 11 42.9482 7.72767 3 -11 -3 -11 33.0357 5.00432 3 11 3 12 196.988 14.2041 3 -11 3 -12 204.456 10.1991 2 -11 -3 -12 201.791 13.8116 2 -11 3 -12 195.090 10.0324 2 11 3 12 205.629 13.8007 2 11 3 12 206.318 12.1014 1 -11 -3 -12 218.692 13.1718 3 11 -3 12 253.905 15.0936 3 11 3 13 60.3691 9.32010 3 11 -3 13 82.9674 10.5762 3 11 3 13 67.8419 7.18812 1 -11 3 -13 60.3208 4.58830 2 -11 -3 -13 58.3284 8.78236 2 11 3 13 59.4693 7.49436 2 -11 -3 -13 79.6718 7.36934 3 11 -3 14 112.065 12.0313 3 11 3 14 122.831 9.20421 1 11 3 14 100.429 11.3014 3 -11 3 -14 121.135 7.10391 2 -11 -3 -14 119.752 10.4561 2 -11 -3 -14 126.691 9.78723 3 11 3 14 115.612 10.2486 2 -11 -3 -15 319.486 19.8054 2 11 3 15 332.859 20.5839 3 -11 3 -15 327.120 16.4750 2 11 3 15 337.006 17.9948 1 11 -3 15 355.051 21.3073 3 -11 -3 -15 327.795 19.2825 3 -11 -3 -16 9.52347 4.90695 3 -11 -3 -16 19.4833 8.07882 2 11 3 16 16.4503 5.90667 1 11 3 16 9.08128 8.76668 3 11 -3 16 19.0589 9.97790 3 -11 -3 -17 72.0651 8.03270 3 -11 -3 -17 88.6741 10.1070 2 11 3 17 73.6833 11.6521 3 11 -3 17 82.2269 12.4314 3 -11 -3 -18 26.1294 6.43810 3 11 3 18 31.8369 10.0084 3 -11 -3 -18 43.0820 9.43185 2 11 -3 18 46.8835 11.4643 3 -11 -3 -19 5.39872 9.25225 2 11 5 -19 238.457 16.6628 2 11 5 -18 34.5484 9.49840 2 11 5 -17 312.191 20.0883 2 11 -5 -17 318.951 19.5860 2 -11 -5 17 348.016 24.5681 1 11 -5 -16 51.8422 7.14307 2 11 5 -16 74.4291 10.3943 2 -11 -5 16 60.0237 13.8897 1 11 -5 -15 219.566 14.3028 2 11 5 -15 202.533 14.7380 2 11 5 -14 464.433 26.3789 2 11 -5 -14 517.155 26.9768 2 11 5 -13 8.85865 7.39958 2 -11 -5 13 8.33650 6.47361 1 11 -5 -13 4.95696 4.23996 2 11 -5 -12 119.684 7.04424 1 11 5 -12 130.113 11.0329 2 -11 -5 12 113.679 11.2006 1 11 -5 -12 120.129 9.64821 2 11 -5 -11 417.747 20.8103 1 11 5 -11 422.516 23.2229 2 -11 -5 11 386.232 24.5720 1 11 -5 -11 437.274 23.4008 2 11 -5 -11 451.486 19.9070 3 11 -5 -11 403.982 19.8092 3 11 -5 -10 213.417 11.4618 3 11 5 -10 240.748 14.8680 2 11 -5 -10 228.729 12.0731 1 -11 -5 10 228.184 15.9131 1 11 -5 -10 248.723 14.3768 2 11 -5 -10 226.393 11.5456 3 11 5 -9 1381.99 66.4998 2 11 -5 -9 1379.91 64.6284 3 -11 -5 9 1399.85 68.8215 1 11 -5 -9 1413.05 64.9156 1 11 -5 -9 1444.25 66.8802 2 11 -5 -8 221.276 11.7683 3 11 -5 -8 207.240 11.6255 1 11 5 -8 197.869 13.6031 2 11 -5 -8 223.158 13.2644 2 -11 -5 8 222.755 15.0307 1 11 5 -7 473.664 25.4209 2 -11 -5 7 486.911 26.9402 1 11 -5 -7 521.292 25.2258 2 11 -5 -7 454.445 23.9627 3 11 5 -7 516.605 28.3504 1 11 -5 -7 473.668 23.5981 1 11 -5 -6 24.7789 3.15342 1 11 5 -6 36.1664 8.45195 1 11 5 -6 41.3081 6.61528 2 11 -5 -6 25.9359 4.13960 2 -11 -5 6 32.0106 5.71851 1 11 5 -5 260.978 16.9048 1 11 5 -5 222.358 14.5341 2 11 -5 -5 233.072 12.9696 1 -11 -5 5 254.274 15.5129 1 11 -5 -5 250.954 13.7376 2 11 5 -4 350.024 20.9503 1 11 5 -4 330.822 18.9840 2 11 -5 -4 357.228 18.1367 2 -11 -5 4 331.411 19.6445 1 11 -5 -4 352.855 17.7945 1 11 -5 -3 948.254 43.7493 1 11 5 -3 917.454 45.9848 1 11 5 -3 881.691 44.3728 2 11 -5 -3 872.986 43.5937 2 -11 -5 3 1027.43 46.8669 3 -11 -5 3 931.932 45.3847 1 -11 -5 3 937.817 45.0589 2 11 5 -2 205.847 15.1114 1 -11 -5 2 225.085 13.7176 1 11 5 -2 234.996 14.1587 2 11 -5 -2 226.951 12.5476 1 11 -5 -2 234.834 12.3944 2 -11 -5 2 234.668 13.8446 2 -11 -5 1 1882.32 92.5167 2 11 5 -1 2042.73 93.2802 1 11 5 -1 2078.05 92.4824 2 11 -5 -1 1957.18 91.1124 2 11 -5 -1 1928.06 91.5522 1 -11 -5 1 2096.65 92.5747 1 11 -5 0 3.47845 2.72990 1 11 5 0 7.33397 6.31977 1 -11 -5 0 6.83986 3.34044 1 11 -5 0 2.35490 2.06435 2 11 5 0 4.54746 5.67265 2 -11 -5 -1 583.931 28.7240 3 11 -5 1 537.366 25.9590 2 11 -5 1 565.342 28.7156 3 -11 -5 -1 534.168 27.0362 1 11 5 1 528.074 28.1038 1 11 -5 1 567.919 27.4276 1 11 -5 2 66.0364 4.11629 2 11 -5 2 56.3024 6.32686 3 -11 -5 -2 62.3161 5.17023 1 11 5 2 60.5534 7.34145 1 -11 -5 -2 82.0461 6.97153 3 11 -5 2 76.2895 6.38409 1 11 -5 3 642.965 31.5445 3 11 -5 3 614.606 27.8803 2 11 5 3 572.393 30.1738 1 -11 -5 -3 560.231 28.8791 1 -11 -5 -3 636.104 31.1082 3 -11 -5 -4 537.320 27.1207 1 11 5 4 563.149 28.1903 1 -11 -5 -4 612.115 30.0079 2 11 -5 4 574.072 29.8007 3 -11 -5 -4 581.381 29.3060 3 11 5 5 1199.76 58.7104 1 -11 -5 -5 1206.30 57.8883 1 -11 -5 -5 1312.40 60.5168 3 11 5 5 1231.30 60.1778 2 11 -5 5 1255.79 60.8835 3 11 5 6 44.8800 6.24349 2 -11 -5 -6 56.4937 4.46496 1 -11 -5 -6 69.3769 9.24687 2 11 5 6 57.6674 6.14165 1 11 -5 6 68.3520 7.35873 3 -11 -5 -6 60.6954 6.77806 3 -11 -5 -7 1270.75 57.5569 2 11 5 7 1142.56 55.4634 1 11 5 7 1167.45 57.5918 2 -11 -5 -7 1229.78 57.4298 3 11 5 8 13.4263 4.35066 2 11 5 8 13.5139 4.32747 1 -11 -5 -8 17.7270 4.36102 3 -11 -5 -9 294.494 16.2813 3 11 5 9 270.337 16.4320 2 -11 -5 -9 279.010 17.1456 2 11 5 9 253.765 13.9273 1 11 -5 9 236.602 18.1079 3 11 -5 10 544.614 28.8914 3 -11 -5 -10 509.531 27.1942 2 11 5 10 472.320 24.0272 1 -11 -5 -10 523.435 26.5735 3 11 5 10 509.783 27.4470 2 11 -5 11-11.8312 9.90969 3 -11 -5 -11 4.98369 8.02732 2 11 5 11 5.28778 3.62917 1 -11 -5 -11-1.34915 4.75115 3 11 5 11 0.56970 4.64560 2 11 5 12 1.22540 4.99746 2 11 -5 12 0.53875 9.67025 3 -11 -5 -12 0.85662 8.75664 2 11 5 12 2.85971 3.35607 1 -11 -5 -12 5.10811 4.45137 3 11 5 13 98.6667 10.1147 2 11 -5 13 144.696 14.4318 3 -11 -5 -13 128.778 9.87912 3 -11 -5 -13 136.086 12.9880 2 11 5 14 33.7364 6.74707 2 11 -5 14 48.0572 12.2545 3 -11 -5 -14 51.9518 10.6348 2 -11 -5 -14 46.5750 6.63464 3 -11 -5 -15 207.286 16.4086 2 11 5 15 181.495 15.4392 2 -11 -5 -15 215.682 14.0033 3 11 -5 15 228.803 18.0053 3 -11 -5 -16 10.1348 5.19670 3 11 7 -16 2.46445 9.37468 2 11 7 -15 75.9047 10.6652 2 11 7 -14 55.4557 10.3064 2 -11 -7 13 4.38429 5.53322 1 11 7 -13 10.2586 9.50166 2 11 -7 -13 13.9178 5.04726 2 11 7 -12 29.3825 10.4182 2 -11 -7 12 35.7118 7.37010 1 11 -7 -12 33.0953 6.05093 2 11 7 -11 263.456 17.6092 2 -11 -7 11 259.509 18.2661 1 11 -7 -11 248.546 16.2059 2 11 7 -10 5.69968 8.05234 2 11 -7 -10 17.0796 5.08265 2 11 -7 -10 6.04932 3.31187 3 -11 -7 10 12.5608 6.52820 1 -11 -7 9 452.563 26.0793 1 11 -7 -9 430.550 23.6826 2 11 7 -9 412.315 23.8444 2 11 7 -8 24.0278 7.50883 2 11 -7 -8 34.5579 3.55722 1 11 -7 -8 41.0181 5.43117 2 -11 -7 8 33.7174 6.99048 1 11 7 -7 716.211 37.6869 2 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4.81904 2 20 2 -3 31.3307 5.02381 3 20 -2 -3 36.7855 5.31003 1 -20 -2 3 37.5503 7.06403 3 20 -2 -3 31.3244 4.25756 3 -20 2 3 41.7562 6.77003 1 20 2 -2 3.11219 7.65251 1 -20 2 2-7.94811 6.41222 3 20 2 -2 15.1701 3.70640 2 -20 -2 2 1.88586 3.09385 1 -20 2 2 4.04448 6.11096 1 20 2 -2-1.80401 3.52100 3 -20 -2 2 5.14534 5.62102 3 20 -2 -2-1.44407 2.89584 3 20 -2 -2-3.78326 3.68341 1 -20 2 1 212.448 14.2762 3 20 -2 -1 225.430 11.7805 2 20 2 -1 233.695 13.3413 2 20 -2 -1 227.211 13.6463 1 20 2 -1 206.252 13.7733 3 -20 2 1 217.844 14.4594 1 20 2 -1 245.573 15.8359 1 -20 -2 1 227.424 13.9015 3 -20 -2 1 222.110 13.3795 1 20 -2 -1 205.127 12.6404 3 -20 2 0 241.024 16.0466 3 -20 -2 0 254.275 14.9135 1 20 -2 0 265.113 13.1382 2 20 2 0 263.763 14.7060 2 20 -2 0 248.641 14.9750 1 20 2 0 251.523 15.6190 3 -20 -2 0 274.664 15.9442 3 20 -2 0 248.268 14.4825 3 20 2 0 263.163 16.9728 1 -20 2 -1 240.674 15.3317 3 -20 -2 -1 223.730 13.5859 1 20 -2 1 234.590 11.5947 2 20 2 1 227.896 13.2900 2 20 2 1 238.292 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46.4836 5.89130 1 20 -4 -3 50.5493 4.77650 2 20 -4 -3 51.7082 5.24911 3 20 4 -2 84.5139 7.51339 2 -20 -4 2 85.8322 7.57103 1 20 -4 -2 86.7521 7.96041 1 20 4 -2 83.1122 11.6221 1 20 -4 -2 85.7479 6.25269 2 -20 -4 2 102.761 10.2339 3 20 -4 -2 93.3727 7.02000 3 20 4 -1 1079.15 53.3274 2 20 4 -1 1122.30 55.5087 1 -20 -4 1 1057.32 53.1757 1 20 -4 -1 1126.40 53.5733 1 20 -4 -1 1095.03 51.1814 2 -20 -4 1 1137.30 53.8448 3 20 -4 -1 1132.70 52.9159 3 -20 -4 0 382.019 21.7181 2 20 4 0 376.502 20.5785 2 20 4 0 379.273 23.1943 1 20 -4 0 361.453 17.7583 2 -20 -4 0 373.568 20.3564 1 -20 -4 0 427.375 21.9266 3 20 -4 0 381.368 20.6155 1 20 -4 0 334.426 19.8843 3 -20 -4 -1 148.295 11.8237 2 20 -4 1 139.371 6.91522 2 20 4 1 151.712 10.4229 2 20 -4 1 144.977 6.95856 2 -20 -4 -1 143.211 12.4338 3 20 4 1 150.401 14.2284 1 20 -4 1 147.163 10.1962 3 -20 -4 -1 153.855 10.1411 1 20 -4 1 143.101 10.1656 1 20 -4 2 336.806 19.6341 1 -20 -4 -2 340.589 19.3150 1 -20 -4 -2 385.361 20.8775 2 20 4 2 353.583 19.8235 2 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32 -2 -5 47.0679 8.55242 1 -32 -2 5 29.5736 5.87542 1 32 -2 -5 29.8927 4.30807 2 32 2 -5 24.1906 5.25154 2 32 -2 -5 33.0268 5.79545 3 32 2 -5 24.4134 13.5382 1 -32 -2 5 38.6006 10.6171 3 -32 2 4 36.5279 10.5709 3 32 -2 -4 39.4763 7.79332 1 32 -2 -4 37.1762 4.40807 2 32 2 -4 49.2446 6.32378 2 -32 -2 4 25.5379 6.01172 1 32 -2 -4 34.4258 5.90968 3 32 2 -4 40.1649 15.2889 1 -32 -2 4 60.1698 12.0150 3 -32 2 4 46.6964 12.0549 1 -32 2 3-4.20558 10.9737 3 32 -2 -3 11.8039 6.11526 1 32 2 -3 9.21513 4.33189 2 32 -2 -3 6.91820 4.43483 3 -32 -2 3 10.0525 5.14182 1 32 2 -3 8.84153 14.0100 1 -32 -2 3 11.8988 10.9854 3 32 2 -2-4.28127 13.5636 1 -32 2 2-6.22343 11.9657 3 -32 -2 2 5.70171 4.51088 1 32 -2 -2-0.76840 5.84250 1 32 2 -2 4.20863 4.18349 2 32 2 -2 2.18603 5.90777 3 32 -2 -2 7.13815 4.53835 3 -32 -2 2 0.53101 11.1902 3 32 2 -1-8.35232 13.7019 1 -32 2 1-7.09245 11.7422 3 32 2 -1 5.01947 3.81008 2 32 -2 -1 7.42831 5.72442 1 -32 -2 1 4.17450 4.56548 1 32 2 -1-1.46730 5.61589 3 32 -2 -1 1.07667 4.06555 3 -32 -2 1 5.44873 11.3895 3 -32 -2 0-6.18090 11.2011 3 32 2 0-11.3757 13.0727 1 -32 2 0-12.6938 12.3687 3 32 2 0 7.88993 4.20203 2 32 2 0 2.95617 5.84534 3 32 -2 0 7.61072 4.95749 3 -32 -2 0-0.60973 5.06128 1 -32 2 -1 46.4562 13.0121 3 32 2 1 89.1311 15.8374 1 -32 -2 -1 63.4163 8.07785 1 32 2 1 66.3641 6.63195 2 32 2 1 41.0020 7.77420 3 32 -2 1 63.2158 7.37083 3 -32 2 -2 4.36238 13.8595 3 32 2 2 21.7087 12.6618 1 32 2 2 12.4202 4.15769 2 32 -2 2 21.4622 5.72549 3 32 2 3 5.41082 3.85580 2 32 -4 -3 70.6335 7.35977 3 32 -4 -2 9.71280 4.51114 3 32 -4 -1 1.01504 4.01339 3 32 -4 0 4.76243 4.24228 3 33 -1 -11 10.0183 4.23416 2 33 -1 -10 17.6086 4.39751 2 33 -1 -9-0.85051 3.96838 2 33 1 -9 4.09575 3.98791 2 -33 -1 8 127.860 13.0400 3 33 -1 -8 103.607 8.42286 2 33 1 -8 128.030 9.32462 2 -33 -1 7 49.7242 10.4099 3 -33 1 7 42.9615 10.7861 3 33 -1 -7 35.6323 4.96112 2 33 1 -7 34.4527 5.33122 2 33 -1 -7 40.6602 6.46017 3 -33 -1 6 155.496 14.2934 3 -33 1 6 152.742 14.0772 3 33 -1 -6 121.009 9.07834 2 33 1 -6 144.952 10.4134 2 33 -1 -6 126.013 10.6392 3 -33 -1 5 23.2754 11.5063 3 -33 1 5 27.3245 10.5021 3 33 -1 -5 22.0895 4.04297 2 33 1 -5 27.0412 5.24632 2 33 -1 -5 20.0953 5.48074 3 -33 -1 4 14.0891 10.6252 3 -33 1 4 26.0166 9.90191 3 33 -1 -4 19.4197 4.08832 2 33 1 -4 22.6223 5.02891 2 33 1 -4 14.5495 5.53160 3 33 -1 -4 23.9653 5.14017 3 -33 -1 3 42.4974 11.4103 3 -33 1 3 20.4783 10.8515 3 33 -1 -3 25.3902 4.08193 2 33 1 -3 22.9776 5.00460 2 33 1 -3 13.1579 5.63345 3 33 -1 -3 37.4189 6.28585 3 -33 1 2 33.2402 11.1722 3 33 1 -2 31.0565 5.25390 2 33 1 -2 25.1401 6.67552 3 33 -1 -2 27.5877 5.94313 3 -33 1 1 8.77418 11.7158 3 33 1 -1 15.0432 4.02141 2 33 1 -1 17.4838 6.05142 3 33 -1 -1 11.4209 4.76110 3 -33 1 0 145.200 16.2721 3 33 1 0 128.455 9.75760 2 33 -1 0 134.427 11.4404 3 33 1 0 130.571 11.8740 3 -33 1 -1-10.2807 12.5116 3 33 1 1 4.47583 3.18554 2 33 -1 1 1.79754 4.97382 3 -33 -3 9 72.9397 11.9341 3 -33 -3 8 145.841 14.4888 3 -33 -3 7 23.9332 11.2038 3 -33 -3 6 85.5318 11.9499 3 33 -3 -5 19.0749 4.79698 3 -33 -3 5 30.1828 11.0473 3 33 3 -4 79.1832 8.02557 2 33 -3 -4 63.7449 7.48233 3 33 3 -3 109.443 9.22426 2 33 -3 -3 85.4089 8.74360 3 33 3 -2 10.5826 4.59663 2 33 -3 -2 3.04774 4.00079 3 33 3 -1 31.0615 5.67838 2 33 -3 -1 30.4974 5.48062 3 33 3 0 17.1118 5.07355 2 33 -3 0 13.9531 4.75303 3 33 3 1-3.42348 4.13057 2 33 3 2 108.673 9.19271 2 33 3 3 12.6818 4.78756 2 34 0 -9 1.32670 3.64902 2 34 0 -8 173.837 11.6065 2 -34 0 7 6.53722 10.4056 3 34 0 -7-0.42017 3.56585 2 34 0 -6 138.517 10.2347 2 34 0 -6 148.012 12.2886 3 -34 0 6 183.186 15.1735 3 -34 0 5 12.3444 10.2748 3 34 0 -5 3.70960 4.19833 2 34 0 -5-0.61471 4.83107 3 -34 0 4 12.1591 9.67432 3 34 0 -4 10.2953 4.16140 2 34 0 -4 13.4827 5.28358 3 -34 0 3 11.4557 10.7616 3 34 0 -3-0.80663 3.57018 2 34 0 -3 0.61888 4.79993 3 34 0 -2 180.696 11.7876 2 34 0 -2 185.585 14.0418 3 -34 0 1 13.4765 12.1516 3 34 0 -1 3.82269 5.26184 3 34 0 0 37.9669 6.83081 3 34 -2 -10 47.3790 5.99612 2 -34 -2 8 212.748 16.5238 3 -34 -2 7-5.10150 10.9044 3 34 2 -6 6.25499 4.21097 2 -34 -2 6 11.9971 10.9566 3 -34 2 5 92.0583 14.2220 3 34 2 -5 114.513 9.51438 2 34 -2 -5 100.981 9.53518 3 -34 2 4 18.9045 10.4981 3 34 2 -4 20.2695 4.97282 2 34 -2 -4 26.8374 5.81040 3 -34 -2 4 40.7265 12.4104 3 -34 2 3 22.1837 12.6673 3 34 2 -3 20.5840 4.73561 2 34 -2 -3 17.2882 5.24894 3 -34 2 2 36.8615 12.0552 3 34 2 -2 54.9052 6.52119 2 34 -2 -2 50.9137 6.85612 3 34 2 -1 2.31974 3.71876 2 34 -2 -1 11.2665 5.18691 3 34 2 0 71.9414 7.18127 2 35 -1 -9 1.72518 3.68115 2 35 1 -7 12.2574 4.12488 2 35 1 -6 6.67204 4.50207 2 35 -1 -6 5.28857 4.83376 3 -35 1 5-5.47267 10.7246 3 35 1 -5-0.96194 4.19322 2 35 -1 -5 1.18148 4.70132 3 -35 1 4 93.0401 14.4440 3 35 1 -4 99.9010 8.71655 2 35 1 -4 90.0556 10.0075 3 35 -1 -4 99.0654 9.54670 3 -35 1 3 5.19260 12.2775 3 35 1 -3 3.54434 4.02186 2 35 1 -3 6.36763 5.59622 3 35 -1 -3 0.59635 4.62716 3 -35 1 2 54.8722 14.5896 3 35 -1 -2 75.6036 8.39850 3 36 0 -7 7.88550 4.23054 2 -36 0 5 31.4137 12.0957 3 36 0 -5-0.66856 5.64718 3 -36 0 4 363.973 22.9626 3 36 0 -4 297.653 19.9780 3 0 0 0 0.00 0.00 0 TITL exp_1 in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 26.257801 7.433419 16.623731 90.0000 99.0889 90.0000 ZERR 14.00 0.000707 0.000195 0.000504 0.0000 0.0027 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 154.00 140.00 14.00 14.00 TREF HKLF 4 END ; _shelx_hkl_checksum 54596 _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n _publcif_funding_html ; ; loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{289c58f7-101e-443d-b2ff-5cad87d27cb5}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{289c58f7-101e-443d-b2ff-5cad87d27cb5}" "_geom_bond_atom_site_label_1" "{289c58f7-101e-443d-b2ff-5cad87d27cb5}" "_publcif_info_datablock.publ_exptl" "{289c58f7-101e-443d-b2ff-5cad87d27cb5}" "_geom_hbond_atom_site_label_D" loop_ _publcif_info_cif.paper_type EE