data_global _audit_creation_date 2018-05-15 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _shelxl_version_number 2013-4 _publ_requested_journal ; European Journal of Chemistry ; _publ_contact_author_name ; Ilkay Gumus ; _publ_contact_author_address ; Department of Chemistry, Faculty of Arts and Science, Mersin University, Mersin, TR 33343, Turkey ; _publ_contact_author_email ; ilkay.gumus@mersin.edu.tr ; _publ_contact_author_fax ; +903243610047 ; _publ_contact_author_phone ; +905385589656 ; _publ_section_title ; Synthesis, characterization and crystal structure of platinum(II) complexes with thiourea derivative ligands ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; data_mo_18_041_4fprpt_0ma_a_d _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H36 F2 N4 O2 Pt S2' _chemical_formula_sum 'C28 H36 F2 N4 O2 Pt S2' _chemical_formula_weight 757.82 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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 'orthorhombic' _space_group_IT_number 43 _space_group_name_H-M_alt 'F d d 2' _space_group_name_Hall 'F 2 -2d' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 26.819(9) _cell_length_b 12.131(5) _cell_length_c 18.880(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6142(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9948 _cell_measurement_temperature 298 _cell_measurement_theta_max 24.674 _cell_measurement_theta_min 3.031 _shelx_estimated_absorpt_T_max 0.600 _shelx_estimated_absorpt_T_min 0.435 _exptl_absorpt_coefficient_mu 4.748 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1113 before and 0.0766 after correction. The Ratio of minimum to maximum transmission is 0.8137. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description BLOCK _exptl_crystal_F_000 3008 _exptl_crystal_recrystallization_method 'obtained by recrystallization of the reaction product from ethanol.' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns.reduction_process narrow-frame _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 45369 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.717 _diffrn_reflns_theta_min 3.029 _diffrn_ambient_temperature 298 _diffrn_detector 'CMOS Area Detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'Bruker D8 VENTURE' _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation.monochromator 'Flat graphite' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source.source 'Fine focus sealed tube' _diffrn_source.type 'Bruker APEX II' _diffrn_source_target Mo _diffrn_standards_number 0 _reflns_Friedel_coverage 0.937 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 2703 _reflns_number_total 3256 _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 V8.38A (17, 2016)' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'SAINT V8.38A (17, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.972 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.079 _refine_ls_abs_structure_details ; Flack x determined using 1194 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.002(6) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 3256 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0267 _refine_ls_restrained_S_all 1.074 _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^)+(0.0212P)^2^+3.3211P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0516 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C7(H7), C8(H8) 2.c Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C14(H14A,H14B,H14C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.2500 0.2500 0.46942(4) 0.04206(11) Uani 1 2 d S T P . . S1 S 0.30705(11) 0.2684(2) 0.38374(13) 0.0660(8) Uani 1 1 d . . . . . F1 F 0.4387(2) 0.3589(6) 0.8070(3) 0.131(3) Uani 1 1 d . . . . . O1 O 0.2980(2) 0.2751(5) 0.5489(4) 0.0558(18) Uani 1 1 d . . . . . N1 N 0.3759(2) 0.2890(6) 0.4917(3) 0.0477(14) Uani 1 1 d . . . . . N2 N 0.4043(2) 0.2679(5) 0.3797(3) 0.0541(16) Uani 1 1 d . . . . . C1 C 0.3649(3) 0.2746(7) 0.4229(4) 0.0469(18) Uani 1 1 d . . . . . C2 C 0.3456(2) 0.2909(6) 0.5458(4) 0.0446(16) Uani 1 1 d . . . . . C3 C 0.3707(2) 0.3134(6) 0.6156(4) 0.0500(17) Uani 1 1 d . . . . . C4 C 0.3427(3) 0.3162(7) 0.6763(4) 0.063(2) Uani 1 1 d . . . . . H4 H 0.3083 0.3077 0.6737 0.076 Uiso 1 1 calc R . . . . C5 C 0.3654(4) 0.3316(8) 0.7420(4) 0.080(3) Uani 1 1 d . . . . . H5 H 0.3467 0.3324 0.7834 0.096 Uiso 1 1 calc R . . . . C6 C 0.4154(5) 0.3456(10) 0.7436(6) 0.087(4) Uani 1 1 d . . . . . C7 C 0.4439(4) 0.3407(12) 0.6844(6) 0.116(5) Uani 1 1 d . . . . . H7 H 0.4785 0.3461 0.6875 0.139 Uiso 1 1 calc R . . . . C8 C 0.4211(3) 0.3277(11) 0.6196(5) 0.089(3) Uani 1 1 d . . . . . H8 H 0.4401 0.3286 0.5784 0.107 Uiso 1 1 calc R . . . . C9 C 0.4008(3) 0.2635(8) 0.3020(4) 0.068(2) Uani 1 1 d . . . . . H9A H 0.3680 0.2891 0.2878 0.081 Uiso 1 1 calc R . . . . H9B H 0.4252 0.3134 0.2819 0.081 Uiso 1 1 calc R . . . . C10 C 0.4087(4) 0.1548(9) 0.2732(6) 0.087(3) Uani 1 1 d . . . . . H10A H 0.3834 0.1045 0.2905 0.104 Uiso 1 1 calc R . . . . H10B H 0.4411 0.1272 0.2876 0.104 Uiso 1 1 calc R . . . . C11 C 0.4059(5) 0.1630(12) 0.1894(6) 0.103(5) Uani 1 1 d . . . . . H11A H 0.4146 0.0931 0.1690 0.155 Uiso 1 1 calc GR . . . . H11B H 0.4289 0.2182 0.1731 0.155 Uiso 1 1 calc GR . . . . H11C H 0.3727 0.1828 0.1754 0.155 Uiso 1 1 calc GR . . . . C12 C 0.4551(2) 0.2716(7) 0.4091(4) 0.057(2) Uani 1 1 d . . . . . H12A H 0.4565 0.3283 0.4453 0.069 Uiso 1 1 calc R . . . . H12B H 0.4782 0.2920 0.3718 0.069 Uiso 1 1 calc R . . . . C13 C 0.4714(3) 0.1638(7) 0.4409(4) 0.065(2) Uani 1 1 d . . . . . H13A H 0.4736 0.1086 0.4039 0.078 Uiso 1 1 calc R . . . . H13B H 0.4467 0.1394 0.4750 0.078 Uiso 1 1 calc R . . . . C14 C 0.5221(3) 0.1746(9) 0.4776(6) 0.092(3) Uani 1 1 d . . . . . H14A H 0.5457 0.2066 0.4454 0.139 Uiso 1 1 calc GR . . . . H14B H 0.5335 0.1030 0.4919 0.139 Uiso 1 1 calc GR . . . . H14C H 0.5188 0.2210 0.5186 0.139 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03146(15) 0.05797(19) 0.03674(15) 0.000 0.000 0.0027(3) S1 0.0326(12) 0.130(2) 0.0356(11) 0.0002(14) 0.0020(9) -0.0065(13) F1 0.120(5) 0.206(8) 0.066(4) -0.037(4) -0.044(4) 0.030(5) O1 0.029(3) 0.097(5) 0.041(3) -0.011(3) 0.003(2) 0.007(3) N1 0.039(3) 0.062(4) 0.042(3) -0.007(3) -0.002(3) 0.001(3) N2 0.036(3) 0.086(5) 0.040(3) 0.001(3) 0.001(2) 0.002(3) C1 0.036(4) 0.062(5) 0.043(4) -0.001(4) 0.003(3) -0.001(3) C2 0.037(4) 0.056(4) 0.040(4) -0.006(3) -0.001(3) 0.007(3) C3 0.047(4) 0.059(5) 0.044(4) -0.007(3) -0.006(3) 0.008(3) C4 0.057(5) 0.088(6) 0.044(4) -0.009(4) -0.009(4) 0.005(4) C5 0.090(7) 0.110(8) 0.040(4) -0.010(4) -0.008(4) 0.004(6) C6 0.088(8) 0.110(9) 0.063(8) -0.027(6) -0.030(6) 0.024(6) C7 0.050(6) 0.222(16) 0.076(7) -0.052(8) -0.021(5) 0.027(7) C8 0.061(6) 0.163(11) 0.044(5) -0.036(6) -0.001(4) 0.005(6) C9 0.054(5) 0.100(8) 0.049(4) -0.001(5) 0.003(4) 0.004(5) C10 0.086(7) 0.091(8) 0.085(7) -0.007(6) -0.011(6) 0.006(6) C11 0.097(10) 0.166(14) 0.047(7) -0.021(7) -0.001(6) 0.017(9) C12 0.033(4) 0.091(6) 0.047(4) 0.006(4) 0.004(3) 0.001(4) C13 0.048(5) 0.082(6) 0.065(5) 0.014(4) 0.002(4) 0.003(4) C14 0.055(5) 0.143(9) 0.079(6) 0.024(7) -0.006(5) 0.019(6) _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 Pt1 S1 2.238(3) 14 ? Pt1 S1 2.238(3) . ? Pt1 O1 2.002(7) . ? Pt1 O1 2.002(7) 14 ? S1 C1 1.721(8) . ? F1 C6 1.360(11) . ? O1 C2 1.292(9) . ? N1 C1 1.342(10) . ? N1 C2 1.307(9) . ? N2 C1 1.338(9) . ? N2 C9 1.470(10) . ? N2 C12 1.471(9) . ? C2 C3 1.503(9) . ? C3 C4 1.370(10) . ? C3 C8 1.365(10) . ? C4 H4 0.9300 . ? C4 C5 1.392(11) . ? C5 H5 0.9300 . ? C5 C6 1.353(13) . ? C6 C7 1.356(14) . ? C7 H7 0.9300 . ? C7 C8 1.378(12) . ? C8 H8 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.442(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.587(14) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.504(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.531(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 S1 Pt1 S1 87.42(15) 14 . ? O1 Pt1 S1 175.9(2) . 14 ? O1 Pt1 S1 94.99(17) . . ? O1 Pt1 S1 175.9(2) 14 . ? O1 Pt1 S1 94.98(17) 14 14 ? O1 Pt1 O1 82.8(4) . 14 ? C1 S1 Pt1 108.1(3) . . ? C2 O1 Pt1 128.6(6) . . ? C2 N1 C1 128.5(7) . . ? C1 N2 C9 124.0(6) . . ? C1 N2 C12 119.9(6) . . ? C9 N2 C12 116.0(6) . . ? N1 C1 S1 128.3(6) . . ? N2 C1 S1 116.6(6) . . ? N2 C1 N1 115.1(6) . . ? O1 C2 N1 130.4(7) . . ? O1 C2 C3 115.4(6) . . ? N1 C2 C3 114.3(6) . . ? C4 C3 C2 119.6(6) . . ? C8 C3 C2 120.9(7) . . ? C8 C3 C4 119.4(7) . . ? C3 C4 H4 119.7 . . ? C3 C4 C5 120.7(8) . . ? C5 C4 H4 119.7 . . ? C4 C5 H5 121.0 . . ? C6 C5 C4 118.0(9) . . ? C6 C5 H5 121.0 . . ? C5 C6 F1 119.4(10) . . ? C5 C6 C7 122.4(9) . . ? C7 C6 F1 118.1(11) . . ? C6 C7 H7 120.5 . . ? C6 C7 C8 119.1(9) . . ? C8 C7 H7 120.5 . . ? C3 C8 C7 120.3(9) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N2 C9 H9A 108.8 . . ? N2 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C10 C9 N2 113.6(8) . . ? C10 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C9 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C9 C10 C11 108.2(10) . . ? H10A C10 H10B 108.4 . . ? C11 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 108.9 . . ? N2 C12 H12B 108.9 . . ? N2 C12 C13 113.2(6) . . ? H12A C12 H12B 107.8 . . ? C13 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C12 C13 C14 111.4(7) . . ? H13A C13 H13B 108.0 . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _shelx_res_file ; TITL mo_18_041_4FPrPt_0ma_a_d.res in Fdd2 REM Old TITL mo_18_041_4FPrPt_0ma_a.hkl REM SHELXT solution in Fdd2 REM R1 0.124, Rweak 0.003, Alpha 0.024, Orientation as input REM Flack x = 0.050 ( 0.010 ) from Parsons' quotients REM Formula found by SHELXT: C26 N10 Pt S4 CELL 0.71073 26.8187 12.1309 18.8796 90 90 90 ZERR 8 0.0089 0.0045 0.0058 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC C H F N O Pt S UNIT 224 288 16 32 16 8 16 L.S. 30 PLAN 5 SIZE 0.12 0.21 0.21 TEMP 24.85 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.021200 3.321100 FVAR 0.10330 PT1 6 0.250000 0.250000 0.469419 10.50000 0.03146 0.05797 = 0.03674 0.00000 0.00000 0.00269 S1 7 0.307054 0.268403 0.383744 11.00000 0.03265 0.12986 = 0.03556 0.00024 0.00197 -0.00650 F1 3 0.438745 0.358854 0.806974 11.00000 0.11975 0.20636 = 0.06567 -0.03660 -0.04449 0.03045 O1 5 0.298042 0.275057 0.548948 11.00000 0.02930 0.09731 = 0.04070 -0.01095 0.00267 0.00716 N1 4 0.375949 0.288981 0.491652 11.00000 0.03881 0.06230 = 0.04191 -0.00657 -0.00249 0.00091 N2 4 0.404338 0.267890 0.379680 11.00000 0.03645 0.08560 = 0.04018 0.00146 0.00059 0.00234 C1 1 0.364932 0.274607 0.422919 11.00000 0.03576 0.06231 = 0.04261 -0.00089 0.00269 -0.00090 C2 1 0.345628 0.290940 0.545829 11.00000 0.03743 0.05622 = 0.04003 -0.00557 -0.00114 0.00732 C3 1 0.370654 0.313441 0.615575 11.00000 0.04694 0.05908 = 0.04393 -0.00721 -0.00629 0.00824 C4 1 0.342745 0.316198 0.676341 11.00000 0.05725 0.08812 = 0.04361 -0.00871 -0.00881 0.00523 AFIX 43 H4 2 0.308333 0.307661 0.673727 11.00000 -1.20000 AFIX 0 C5 1 0.365381 0.331650 0.741961 11.00000 0.08959 0.11044 = 0.03966 -0.01044 -0.00839 0.00424 AFIX 43 H5 2 0.346660 0.332391 0.783423 11.00000 -1.20000 AFIX 0 C6 1 0.415416 0.345553 0.743616 11.00000 0.08799 0.10965 = 0.06342 -0.02732 -0.03000 0.02371 C7 1 0.443945 0.340737 0.684406 11.00000 0.04986 0.22225 = 0.07579 -0.05213 -0.02070 0.02733 AFIX 43 H7 2 0.478467 0.346148 0.687497 11.00000 -1.20000 AFIX 0 C8 1 0.421065 0.327711 0.619568 11.00000 0.06143 0.16315 = 0.04368 -0.03621 -0.00090 0.00497 AFIX 43 H8 2 0.440058 0.328648 0.578358 11.00000 -1.20000 AFIX 0 C9 1 0.400756 0.263470 0.302037 11.00000 0.05417 0.09975 = 0.04930 -0.00096 0.00340 0.00369 AFIX 23 H9A 2 0.367985 0.289096 0.287839 11.00000 -1.20000 H9B 2 0.425201 0.313421 0.281942 11.00000 -1.20000 AFIX 0 C10 1 0.408737 0.154790 0.273203 11.00000 0.08562 0.09099 = 0.08460 -0.00741 -0.01132 0.00612 AFIX 23 H10A 2 0.383393 0.104532 0.290547 11.00000 -1.20000 H10B 2 0.441130 0.127153 0.287591 11.00000 -1.20000 AFIX 0 C11 1 0.405950 0.163033 0.189395 11.00000 0.09664 0.16613 = 0.04742 -0.02091 -0.00077 0.01670 AFIX 137 H11A 2 0.414558 0.093102 0.168976 11.00000 -1.50000 H11B 2 0.428896 0.218220 0.173094 11.00000 -1.50000 H11C 2 0.372708 0.182765 0.175425 11.00000 -1.50000 AFIX 0 C12 1 0.455072 0.271629 0.409128 11.00000 0.03343 0.09148 = 0.04667 0.00581 0.00351 0.00054 AFIX 23 H12A 2 0.456508 0.328341 0.445291 11.00000 -1.20000 H12B 2 0.478186 0.291982 0.371836 11.00000 -1.20000 AFIX 0 C13 1 0.471393 0.163797 0.440885 11.00000 0.04826 0.08244 = 0.06534 0.01369 0.00230 0.00323 AFIX 23 H13A 2 0.473591 0.108551 0.403873 11.00000 -1.20000 H13B 2 0.446700 0.139389 0.474993 11.00000 -1.20000 AFIX 0 C14 1 0.522056 0.174604 0.477604 11.00000 0.05545 0.14253 = 0.07920 0.02409 -0.00586 0.01899 AFIX 137 H14A 2 0.545668 0.206644 0.445405 11.00000 -1.50000 H14B 2 0.533499 0.102986 0.491880 11.00000 -1.50000 H14C 2 0.518770 0.220957 0.518551 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_18_041_4FPrPt_0ma_a_d.res in Fdd2 REM R1 = 0.0267 for 2703 Fo > 4sig(Fo) and 0.0425 for all 3256 data REM 179 parameters refined using 1 restraints END WGHT 0.0212 3.3474 REM Highest difference peak 0.972, deepest hole -0.922, 1-sigma level 0.079 Q1 1 0.5000 0.5000 0.7200 10.50000 0.05 0.97 Q2 1 0.4064 0.2541 0.2502 11.00000 0.05 0.36 Q3 1 0.4083 0.2477 0.6880 11.00000 0.05 0.34 Q4 1 0.2743 0.1482 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167.98 39.60 33 1 -1 124.89 49.40 -33 1 1 81.59 33.60 -33 1 1 136.59 50.39 -33 -1 -1 124.59 36.60 -33 -1 -1 130.59 52.49 33 1 -1 147.49 40.10 33 -1 1 140.59 45.10 33 1 -1 173.28 47.10 33 1 1 128.29 36.40 -33 1 -1 190.48 52.79 33 -1 -1 141.89 45.60 33 1 1 121.09 50.59 -33 1 -1 119.19 38.30 -33 -1 1 65.79 47.70 -33 -1 1 132.49 37.20 33 1 1 82.79 39.50 33 -1 -1 153.58 50.69 -33 3 1 87.99 41.10 33 -3 1 130.19 48.20 33 -3 1 209.78 53.99 33 -3 1 41.10 44.60 -33 -3 -1 173.18 47.20 33 3 -1 88.59 50.89 -33 3 1 211.68 57.29 -33 -3 -1 82.79 36.00 -33 3 -1 109.19 52.89 -33 -3 1 80.89 44.70 33 3 1 90.19 41.40 -33 3 -1 175.68 42.20 33 3 1 85.29 45.00 33 -3 -1 152.88 51.99 33 -3 -1 24.60 44.70 33 -3 -1 99.89 41.80 -33 -3 1 119.79 35.00 -33 1 3 49.30 46.00 33 1 -3 130.39 43.80 33 -1 3 68.79 48.70 -33 1 3 63.49 31.90 -33 -1 -3 82.79 49.50 -33 -1 -3 94.69 36.00 33 -1 3 44.10 44.60 33 -1 3 58.49 42.20 33 1 -3 96.89 49.10 -33 1 -3 91.49 39.50 -33 -1 3 72.69 43.00 33 1 3 107.09 49.10 -33 -1 3 60.49 31.20 33 -1 -3 146.29 45.40 33 -1 -3 71.49 47.60 33 1 3 68.89 41.00 33 1 3 137.89 44.50 -33 1 -3 -27.50 47.80 -33 -3 -3 -1.00 39.60 -33 3 3 48.00 49.50 33 -3 3 -7.80 34.30 33 3 3 91.19 45.60 -33 3 -3 10.80 50.99 33 -3 -3 2.60 43.30 -33 -3 3 32.20 40.90 -33 1 5 25.30 48.40 -33 -1 -5 84.69 51.59 -33 -1 -5 62.39 36.90 -33 1 5 49.70 25.80 33 1 -5 74.99 52.09 33 1 -5 26.30 40.60 33 -1 5 11.70 42.00 33 1 5 46.60 48.70 -33 1 -5 117.49 51.19 -33 -1 5 38.50 46.00 33 1 5 58.19 41.70 -33 1 -5 33.60 40.00 33 -1 -5 43.30 44.00 33 -1 -5 -19.00 42.70 -33 -1 5 93.69 28.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78574 _olex2_exptl_crystal_mounting_method 'coated with Paratone oil and mounted onto a Nylon loop' _olex2_submission_special_instructions 'No special instructions were received'