data_[(6Dipp)Pd(cinn)]+BF4- _audit_creation_date 2019-07-01 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 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 ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C37 H48.89 N2 Pd, B F4, C H Cl3' _chemical_formula_sum 'C38 H49.88 B Cl3 F4 N2 Pd' _chemical_formula_weight 834.24 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2879(6) _cell_length_b 12.5324(7) _cell_length_c 25.7400(14) _cell_angle_alpha 90 _cell_angle_beta 101.1710(10) _cell_angle_gamma 90 _cell_volume 3888.8(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9947 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 28.24 _cell_measurement_theta_min 2.29 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6802 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0638 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.9117. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1720 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_unetI/netI 0.0440 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 79902 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.536 _diffrn_reflns_theta_min 1.613 _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \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 9521 _reflns_number_total 11877 _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 ? _computing_data_collection ? _computing_data_reduction ? _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 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 1.823 _refine_diff_density_min -2.107 _refine_diff_density_rms 0.122 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 541 _refine_ls_number_reflns 11877 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0843 _refine_ls_restrained_S_all 1.127 _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^)+(0.0301P)^2^+28.3365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1769 _refine_ls_wR_factor_ref 0.1854 _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. Restrained distances Cl1-C1S \\sim Cl3S-C1S with sigma of 0.005 C31A-C30A \\sim C31-C30 with sigma of 0.005 F4A-F2A \\sim F4-F2 \\sim F3-F2 \\sim F3A-F2A with sigma of 0.01 B1-F4A \\sim B1-F4 \\sim B1-F3 \\sim B1-F3A \\sim B1-F2A \\sim B1-F2 \\sim B1-F1 with sigma of 0.005 3. Uiso/Uaniso restraints and constraints Cl1 \\sim Cl3S: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005 F4A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005 C32 \\sim C33 \\sim C33A \\sim C34 \\sim C34A \\sim C35A \\sim C35 \\sim C36 \\sim C36A \\sim C37 \\sim C37A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005 4. Rigid body (RIGU) restrains Cl3S, Cl1 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H1SA)=Sof(Cl1)=1-FVAR(1) Sof(H1S)=Sof(H31)=Sof(Cl3S)=FVAR(1) Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=1-FVAR(2) Sof(C31)=Sof(C30)=Sof(H30)=FVAR(2) Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(3) Sof(F2)=Sof(F3)=Sof(F4)=FVAR(3) Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)= Sof(H36A)=Sof(C37A)=Sof(H37A)=1-FVAR(4) Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)= Sof(C37)=Sof(H37)=FVAR(4) 6.a Ternary CH refined with riding coordinates: C23(H23), C26(H26), C14(H14), C11(H11), C1S(H1S), C1S(H1SA), C31(H31), C30(H30), C30A(H30A), C31A(H31A) 6.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B), C29(H29A,H29B) 6.c Aromatic/amide H refined with riding coordinates: C21(H21), C20(H20), C9(H9), C19(H19), C7(H7), C8(H8), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C37A(H37A) 6.d Fitted hexagon refined as free rotating group: C32(C33,C34,C35,C36,C37) 6.e Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C28(H28A,H28B, H28C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C13(H13A, H13B,H13C) ; _atom_sites_solution_hydrogens geom _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 Pd1 Pd 0.66019(3) 0.69799(3) 0.35840(2) 0.02908(10) Uani 1 1 d . . . . . N1 N 0.6119(3) 0.7330(3) 0.45373(14) 0.0201(7) Uani 1 1 d . . . . . N2 N 0.7443(3) 0.8617(3) 0.45068(14) 0.0207(7) Uani 1 1 d . . . . . C3 C 0.6833(3) 0.7804(3) 0.42824(16) 0.0191(8) Uani 1 1 d . . . . . F1 F 0.6369(5) 0.7670(4) 0.63372(18) 0.0828(16) Uani 1 1 d D . . . . C10 C 0.7815(4) 0.9992(4) 0.38876(19) 0.0311(10) Uani 1 1 d . . . . . C5 C 0.8213(4) 0.9147(4) 0.42295(18) 0.0250(9) Uani 1 1 d . . . . . C17 C 0.5493(3) 0.6510(3) 0.42197(17) 0.0196(8) Uani 1 1 d . . . . . C21 C 0.3866(4) 0.5970(5) 0.3591(2) 0.0324(11) Uani 1 1 d . . . . . H21 H 0.320073 0.613910 0.334960 0.039 Uiso 1 1 calc R . . . . C4 C 0.7352(4) 0.9026(4) 0.50378(18) 0.0266(9) Uani 1 1 d . . . . . H4A H 0.752447 0.979824 0.505998 0.032 Uiso 1 1 calc R . . . . H4B H 0.789290 0.865417 0.531358 0.032 Uiso 1 1 calc R . . . . C20 C 0.4194(4) 0.4907(4) 0.3663(2) 0.0302(10) Uani 1 1 d . . . . . H20 H 0.373861 0.435827 0.348200 0.036 Uiso 1 1 calc R . . . . C22 C 0.4493(4) 0.6789(4) 0.38656(18) 0.0251(9) Uani 1 1 d . . . . . C18 C 0.5856(3) 0.5433(3) 0.42833(17) 0.0214(8) Uani 1 1 d . . . . . C6 C 0.9321(4) 0.8813(4) 0.4332(2) 0.0323(11) Uani 1 1 d . . . . . C23 C 0.6935(4) 0.5121(4) 0.46501(18) 0.0247(9) Uani 1 1 d . . . . . H23 H 0.725183 0.577437 0.484552 0.030 Uiso 1 1 calc R . . . . C9 C 0.8594(5) 1.0512(5) 0.3647(2) 0.0428(14) Uani 1 1 d . . . . . H9 H 0.835458 1.108032 0.340749 0.051 Uiso 1 1 calc R . . . . C19 C 0.5181(4) 0.4649(4) 0.39978(19) 0.0287(10) Uani 1 1 d . . . . . H19 H 0.540607 0.392331 0.403451 0.034 Uiso 1 1 calc R . . . . C2 C 0.5883(4) 0.7663(4) 0.50537(18) 0.0246(9) Uani 1 1 d . . . . . H2A H 0.632767 0.723355 0.534130 0.030 Uiso 1 1 calc R . . . . H2B H 0.508772 0.755442 0.506023 0.030 Uiso 1 1 calc R . . . . C1 C 0.6181(4) 0.8842(4) 0.51330(19) 0.0256(9) Uani 1 1 d . . . . . H1A H 0.564794 0.927949 0.488315 0.031 Uiso 1 1 calc R . . . . H1B H 0.613663 0.905966 0.549803 0.031 Uiso 1 1 calc R . . . . C7 C 1.0051(5) 0.9388(5) 0.4078(2) 0.0426(14) Uani 1 1 d . . . . . H7 H 1.081180 0.918942 0.413889 0.051 Uiso 1 1 calc R . . . . C25 C 0.6754(4) 0.4295(5) 0.5054(2) 0.0351(11) Uani 1 1 d . . . . . H25A H 0.618790 0.455148 0.524531 0.053 Uiso 1 1 calc GR . . . . H25B H 0.745040 0.417396 0.530595 0.053 Uiso 1 1 calc GR . . . . H25C H 0.650498 0.362444 0.487367 0.053 Uiso 1 1 calc GR . . . . C8 C 0.9698(5) 1.0227(5) 0.3744(2) 0.0457(15) Uani 1 1 d . . . . . H8 H 1.021123 1.060778 0.358181 0.055 Uiso 1 1 calc R . . . . C27 C 0.3962(5) 0.8279(5) 0.3208(2) 0.0431(13) Uani 1 1 d . . . . . H27A H 0.468248 0.823699 0.309956 0.065 Uiso 1 1 calc GR . . . . H27B H 0.368779 0.901454 0.316947 0.065 Uiso 1 1 calc GR . . . . H27C H 0.343297 0.780572 0.298494 0.065 Uiso 1 1 calc GR . . . . C26 C 0.4093(4) 0.7933(4) 0.3790(2) 0.0294(9) Uani 1 1 d . . . . . H26 H 0.466825 0.840088 0.400630 0.035 Uiso 1 1 calc R . . . . C14 C 0.6609(4) 1.0357(5) 0.3780(2) 0.0384(12) Uani 1 1 d . . . . . H14 H 0.617817 0.982475 0.394708 0.046 Uiso 1 1 calc R . . . . C11 C 0.9725(4) 0.7866(4) 0.4682(2) 0.0374(12) Uani 1 1 d . . . . . H11 H 0.913162 0.766659 0.488113 0.045 Uiso 1 1 calc R . . . . C1S C 0.9314(5) 0.6113(6) 0.6509(2) 0.0466(14) Uani 1 1 d D . . . . H1S H 0.878847 0.659227 0.664935 0.056 Uiso 0.661(13) 1 calc R . P A 1 H1SA H 0.886983 0.674236 0.658468 0.056 Uiso 0.339(13) 1 calc R . P A 2 C24 C 0.7781(4) 0.4705(5) 0.4332(2) 0.0395(12) Uani 1 1 d . . . . . H24A H 0.750692 0.404013 0.415258 0.059 Uiso 1 1 calc GR . . . . H24B H 0.849020 0.457172 0.457138 0.059 Uiso 1 1 calc GR . . . . H24C H 0.788564 0.523880 0.406725 0.059 Uiso 1 1 calc GR . . . . C28 C 0.2998(5) 0.8112(5) 0.3980(3) 0.0442(14) Uani 1 1 d . . . . . H28A H 0.243532 0.761815 0.379477 0.066 Uiso 1 1 calc GR . . . . H28B H 0.274853 0.884826 0.390324 0.066 Uiso 1 1 calc GR . . . . H28C H 0.311090 0.798418 0.436191 0.066 Uiso 1 1 calc GR . . . . C29 C 0.7648(5) 0.7547(6) 0.3095(2) 0.0457(15) Uani 1 1 d . . . . . H29A H 0.736122 0.814902 0.285880 0.055 Uiso 1 1 calc R . . B . H29B H 0.844092 0.762407 0.326113 0.055 Uiso 1 1 calc R . . B . C16 C 0.6117(6) 1.0368(6) 0.3183(2) 0.0510(16) Uani 1 1 d . . . . . H16A H 0.648462 1.092057 0.300994 0.077 Uiso 1 1 calc GR . . . . H16B H 0.532021 1.052053 0.312855 0.077 Uiso 1 1 calc GR . . . . H16C H 0.623099 0.967039 0.303039 0.077 Uiso 1 1 calc GR . . . . C12 C 1.0772(5) 0.8138(5) 0.5083(3) 0.0498(15) Uani 1 1 d . . . . . H12A H 1.138676 0.825506 0.489788 0.075 Uiso 1 1 calc GR . . . . H12B H 1.095536 0.754618 0.533401 0.075 Uiso 1 1 calc GR . . . . H12C H 1.064617 0.878653 0.527580 0.075 Uiso 1 1 calc GR . . . . C15 C 0.6467(5) 1.1429(6) 0.4027(3) 0.0545(17) Uani 1 1 d . . . . . H15A H 0.666890 1.137004 0.441352 0.082 Uiso 1 1 calc GR . . . . H15B H 0.569264 1.165846 0.392601 0.082 Uiso 1 1 calc GR . . . . H15C H 0.694897 1.195499 0.390255 0.082 Uiso 1 1 calc GR . . . . C31 C 0.6215(6) 0.6295(6) 0.2765(2) 0.0290(17) Uani 0.775(15) 1 d D . P C 1 H31 H 0.580134 0.680957 0.250214 0.035 Uiso 0.661(13) 1 calc R . P A 1 C13 C 0.9930(6) 0.6919(6) 0.4349(4) 0.069(2) Uani 1 1 d . . . . . H13A H 0.925851 0.676933 0.408491 0.103 Uiso 1 1 calc GR . . . . H13B H 1.011998 0.629398 0.457714 0.103 Uiso 1 1 calc GR . . . . H13C H 1.054360 0.708152 0.416893 0.103 Uiso 1 1 calc GR . . . . C30 C 0.7318(7) 0.6568(7) 0.2920(3) 0.0334(19) Uani 0.775(15) 1 d D . P C 1 H30 H 0.788329 0.598482 0.296391 0.040 Uiso 0.775(15) 1 calc R . P C 1 B1 B 0.7119(4) 0.8329(4) 0.66365(19) 0.0462(16) Uani 1 1 d D . . . . Cl2S Cl 1.06849(14) 0.65716(17) 0.66943(8) 0.0654(5) Uani 1 1 d . . . . . Cl1S Cl 0.8944(2) 0.59950(19) 0.58227(8) 0.0766(6) Uani 1 1 d . . . . . F2 F 0.7930(6) 0.7693(6) 0.6918(3) 0.096(2) Uani 0.697(6) 1 d D U P D 1 F3 F 0.6733(6) 0.8877(6) 0.7025(3) 0.0817(18) Uani 0.697(6) 1 d D U P D 1 F4 F 0.7610(6) 0.9036(6) 0.6352(3) 0.0833(19) Uani 0.697(6) 1 d D U P D 1 C32 C 0.5745(4) 0.5196(4) 0.26934(19) 0.0372(10) Uani 1 1 d . U . . . C33 C 0.6420(5) 0.4331(5) 0.2875(3) 0.0375(16) Uani 0.508(10) 1 d G U P C 1 H33 H 0.717514 0.444286 0.303612 0.045 Uiso 0.508(10) 1 calc R . P C 1 C34 C 0.5991(9) 0.3302(4) 0.2822(4) 0.0408(16) Uani 0.508(10) 1 d G U P C 1 H34 H 0.645258 0.271057 0.294576 0.049 Uiso 0.508(10) 1 calc R . P C 1 C35 C 0.4887(9) 0.3138(5) 0.2586(4) 0.0428(16) Uani 0.508(10) 1 d G U P C 1 H35 H 0.459363 0.243461 0.254933 0.051 Uiso 0.508(10) 1 calc R . P C 1 C36 C 0.4212(6) 0.4003(8) 0.2404(4) 0.0448(17) Uani 0.508(10) 1 d G U P C 1 H36 H 0.345721 0.389096 0.224326 0.054 Uiso 0.508(10) 1 calc R . P C 1 C37 C 0.4641(4) 0.5032(6) 0.2458(3) 0.0423(16) Uani 0.508(10) 1 d G U P C 1 H37 H 0.417974 0.562326 0.233361 0.051 Uiso 0.508(10) 1 calc R . P C 1 Cl3S Cl 0.9271(5) 0.4795(4) 0.6762(2) 0.0752(14) Uani 0.661(13) 1 d D U P A 1 Cl1 Cl 0.8976(8) 0.5132(9) 0.6945(4) 0.072(2) Uani 0.339(13) 1 d D U P A 2 C30A C 0.682(2) 0.6734(16) 0.2808(9) 0.029(6) Uani 0.225(15) 1 d D . P C 2 H30A H 0.622462 0.700034 0.251424 0.035 Uiso 0.225(15) 1 calc R . P C 2 C31A C 0.6788(18) 0.5673(15) 0.2946(7) 0.027(6) Uani 0.225(15) 1 d D . P C 2 H31A H 0.748280 0.523938 0.299224 0.032 Uiso 0.225(15) 1 calc R . P C 2 F2A F 0.7435(13) 0.8319(14) 0.7168(3) 0.094(2) Uani 0.303(6) 1 d D U P D 2 F3A F 0.6591(13) 0.9267(8) 0.6489(6) 0.084(2) Uani 0.303(6) 1 d D U P D 2 F4A F 0.8009(10) 0.8397(16) 0.6398(6) 0.083(2) Uani 0.303(6) 1 d D U P D 2 C33A C 0.6085(12) 0.4079(12) 0.2821(5) 0.0413(15) Uani 0.492(10) 1 d . U P C 2 H33A H 0.682107 0.394653 0.300323 0.050 Uiso 0.492(10) 1 calc R . P C 2 C34A C 0.5428(14) 0.3273(11) 0.2696(5) 0.0443(16) Uani 0.492(10) 1 d . U P C 2 H34A H 0.570389 0.257192 0.277528 0.053 Uiso 0.492(10) 1 calc R . P C 2 C35A C 0.4355(13) 0.3407(12) 0.2453(5) 0.0432(17) Uani 0.492(10) 1 d . U P C 2 H35A H 0.388830 0.280504 0.235948 0.052 Uiso 0.492(10) 1 calc R . P C 2 C36A C 0.3935(11) 0.4455(12) 0.2341(5) 0.0413(16) Uani 0.492(10) 1 d . U P C 2 H36A H 0.318007 0.456824 0.218144 0.050 Uiso 0.492(10) 1 calc R . P C 2 C37A C 0.4656(11) 0.5312(12) 0.2471(5) 0.0408(16) Uani 0.492(10) 1 d . U P C 2 H37A H 0.437161 0.601331 0.240117 0.049 Uiso 0.492(10) 1 calc R . P C 2 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 Pd1 0.02562(17) 0.0390(2) 0.02591(17) -0.00907(16) 0.01320(13) -0.01198(16) N1 0.0198(16) 0.0211(17) 0.0215(16) -0.0017(13) 0.0091(13) -0.0027(13) N2 0.0199(16) 0.0193(17) 0.0250(17) -0.0045(14) 0.0097(14) -0.0027(13) C3 0.0196(18) 0.0163(19) 0.0237(19) -0.0011(14) 0.0099(15) -0.0004(14) F1 0.116(4) 0.074(3) 0.061(3) -0.002(2) 0.021(3) -0.045(3) C10 0.032(2) 0.036(3) 0.026(2) -0.0025(19) 0.0082(19) -0.010(2) C5 0.023(2) 0.026(2) 0.029(2) -0.0064(17) 0.0118(17) -0.0100(17) C17 0.0141(17) 0.023(2) 0.0238(19) 0.0012(16) 0.0093(15) -0.0013(15) C21 0.019(2) 0.045(3) 0.033(2) 0.001(2) 0.0053(18) -0.008(2) C4 0.028(2) 0.028(2) 0.026(2) -0.0077(18) 0.0107(17) -0.0058(18) C20 0.027(2) 0.033(3) 0.032(2) -0.008(2) 0.0098(19) -0.0127(19) C22 0.0205(19) 0.028(2) 0.028(2) 0.0015(17) 0.0076(16) -0.0010(16) C18 0.0201(19) 0.021(2) 0.026(2) 0.0001(16) 0.0109(16) -0.0005(15) C6 0.023(2) 0.034(3) 0.043(3) -0.011(2) 0.015(2) -0.0057(19) C23 0.021(2) 0.023(2) 0.031(2) 0.0022(17) 0.0077(17) 0.0008(16) C9 0.052(3) 0.049(3) 0.030(3) -0.001(2) 0.014(2) -0.024(3) C19 0.031(2) 0.026(2) 0.033(2) -0.0047(19) 0.0137(19) -0.0043(18) C2 0.030(2) 0.023(2) 0.025(2) -0.0042(16) 0.0147(17) -0.0030(17) C1 0.030(2) 0.021(2) 0.029(2) -0.0048(17) 0.0145(18) 0.0013(17) C7 0.032(3) 0.050(3) 0.053(3) -0.015(3) 0.026(2) -0.012(2) C25 0.031(2) 0.040(3) 0.037(3) 0.012(2) 0.011(2) 0.003(2) C8 0.046(3) 0.055(4) 0.044(3) -0.012(3) 0.029(3) -0.026(3) C27 0.037(3) 0.047(3) 0.045(3) 0.014(3) 0.009(2) 0.006(2) C26 0.022(2) 0.029(2) 0.037(2) 0.005(2) 0.0053(18) -0.0001(18) C14 0.031(3) 0.046(3) 0.035(3) 0.014(2) 0.001(2) -0.009(2) C11 0.024(2) 0.029(3) 0.061(3) -0.005(2) 0.014(2) 0.0025(19) C1S 0.035(3) 0.057(4) 0.045(3) -0.010(3) -0.001(2) -0.008(3) C24 0.028(2) 0.048(3) 0.045(3) 0.006(3) 0.015(2) 0.008(2) C28 0.034(3) 0.045(3) 0.059(4) 0.011(3) 0.022(3) 0.010(2) C29 0.046(3) 0.064(4) 0.033(3) -0.011(3) 0.022(2) -0.026(3) C16 0.058(4) 0.047(4) 0.041(3) 0.009(3) -0.008(3) -0.006(3) C12 0.053(4) 0.038(3) 0.058(4) -0.016(3) 0.006(3) -0.003(3) C15 0.040(3) 0.072(5) 0.049(4) -0.009(3) 0.003(3) 0.007(3) C31 0.030(4) 0.036(4) 0.022(3) -0.001(2) 0.009(2) -0.008(3) C13 0.049(4) 0.044(4) 0.102(6) -0.034(4) -0.012(4) 0.003(3) C30 0.026(4) 0.049(5) 0.030(4) -0.008(3) 0.017(3) -0.007(4) B1 0.041(4) 0.048(4) 0.051(4) 0.003(3) 0.011(3) 0.004(3) Cl2S 0.0412(8) 0.0750(12) 0.0783(12) -0.0256(10) 0.0072(8) -0.0155(8) Cl1S 0.0888(15) 0.0797(14) 0.0487(10) -0.0191(10) -0.0178(9) 0.0162(12) F2 0.106(4) 0.086(4) 0.085(4) -0.004(3) -0.008(3) 0.037(3) F3 0.085(4) 0.075(4) 0.093(4) -0.025(3) 0.037(3) 0.001(3) F4 0.084(4) 0.090(4) 0.076(3) 0.015(3) 0.014(3) -0.032(3) C32 0.042(2) 0.046(2) 0.0266(19) -0.0091(18) 0.0138(17) -0.012(2) C33 0.043(3) 0.041(3) 0.030(3) -0.012(3) 0.012(3) -0.013(3) C34 0.046(3) 0.044(3) 0.034(3) -0.009(3) 0.013(3) -0.011(3) C35 0.048(4) 0.045(3) 0.036(3) -0.008(3) 0.012(3) -0.013(3) C36 0.050(3) 0.049(4) 0.036(3) -0.006(3) 0.010(3) -0.012(3) C37 0.048(3) 0.049(4) 0.031(3) -0.005(3) 0.010(2) -0.010(3) Cl3S 0.078(3) 0.073(2) 0.074(3) 0.012(2) 0.0104(19) -0.018(2) Cl1 0.065(4) 0.079(4) 0.067(4) 0.010(3) 0.006(3) -0.021(3) C30A 0.012(11) 0.055(16) 0.024(11) -0.004(10) 0.010(9) -0.002(12) C31A 0.028(11) 0.038(12) 0.015(9) -0.008(8) 0.004(7) 0.000(9) F2A 0.100(5) 0.087(5) 0.090(4) -0.006(4) 0.008(4) 0.009(4) F3A 0.088(4) 0.077(4) 0.087(4) -0.012(4) 0.021(4) -0.009(4) F4A 0.085(5) 0.081(5) 0.082(4) 0.007(4) 0.015(4) 0.000(4) C33A 0.044(3) 0.048(3) 0.032(3) -0.012(3) 0.010(3) -0.006(3) C34A 0.051(4) 0.046(3) 0.036(3) -0.008(3) 0.009(3) -0.003(3) C35A 0.050(3) 0.046(3) 0.035(3) -0.007(3) 0.011(3) -0.010(3) C36A 0.044(3) 0.048(4) 0.033(3) -0.002(3) 0.009(3) -0.008(3) C37A 0.047(3) 0.047(4) 0.030(3) -0.004(3) 0.012(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C3 2.045(4) . ? Pd1 C17 2.397(4) . ? Pd1 C29 2.090(5) . ? Pd1 C31 2.239(6) . ? Pd1 C30 2.131(7) . ? Pd1 C30A 2.09(2) . ? Pd1 C31A 2.361(19) . ? N1 C3 1.333(5) . ? N1 C17 1.439(5) . ? N1 C2 1.475(5) . ? N2 C3 1.328(5) . ? N2 C5 1.452(5) . ? N2 C4 1.484(5) . ? F1 B1 1.360(4) . ? C10 C5 1.403(7) . ? C10 C9 1.399(7) . ? C10 C14 1.524(8) . ? C5 C6 1.400(7) . ? C17 C22 1.425(6) . ? C17 C18 1.422(6) . ? C21 H21 0.9500 . ? C21 C20 1.394(8) . ? C21 C22 1.390(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C1 1.523(6) . ? C20 H20 0.9500 . ? C20 C19 1.383(7) . ? C22 C26 1.517(7) . ? C18 C23 1.523(6) . ? C18 C19 1.398(6) . ? C6 C7 1.407(7) . ? C6 C11 1.514(8) . ? C23 H23 1.0000 . ? C23 C25 1.515(7) . ? C23 C24 1.534(7) . ? C9 H9 0.9500 . ? C9 C8 1.378(9) . ? C19 H19 0.9500 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C1 1.526(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C7 H7 0.9500 . ? C7 C8 1.374(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C8 H8 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 C26 1.537(7) . ? C26 H26 1.0000 . ? C26 C28 1.534(7) . ? C14 H14 1.0000 . ? C14 C16 1.537(8) . ? C14 C15 1.511(9) . ? C11 H11 1.0000 . ? C11 C12 1.524(8) . ? C11 C13 1.513(8) . ? C1S H1S 1.0000 . ? C1S H1SA 1.0000 . ? C1S Cl2S 1.756(6) . ? C1S Cl1S 1.742(6) . ? C1S Cl3S 1.780(7) . ? C1S Cl1 1.768(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.342(10) . ? C29 C30A 1.53(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C31 H31 1.0000 . ? C31 C30 1.380(10) . ? C31 C32 1.491(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C30 H30 1.0000 . ? B1 F2 1.369(4) . ? B1 F3 1.371(4) . ? B1 F4 1.362(4) . ? B1 F2A 1.349(5) . ? B1 F3A 1.361(5) . ? B1 F4A 1.357(5) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C32 C31A 1.45(2) . ? C32 C33A 1.479(15) . ? C32 C37A 1.358(15) . ? C33 H33 0.9500 . ? C33 C34 1.3900 . ? C34 H34 0.9500 . ? C34 C35 1.3900 . ? C35 H35 0.9500 . ? C35 C36 1.3900 . ? C36 H36 0.9500 . ? C36 C37 1.3900 . ? C37 H37 0.9500 . ? C30A H30A 1.0000 . ? C30A C31A 1.379(10) . ? C31A H31A 1.0000 . ? C33A H33A 0.9500 . ? C33A C34A 1.294(18) . ? C34A H34A 0.9500 . ? C34A C35A 1.355(19) . ? C35A H35A 0.9500 . ? C35A C36A 1.421(19) . ? C36A H36A 0.9500 . ? C36A C37A 1.391(17) . ? C37A H37A 0.9500 . ? 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 C3 Pd1 C17 61.61(15) . . ? C3 Pd1 C29 111.13(19) . . ? C3 Pd1 C31 171.4(2) . . ? C3 Pd1 C30 144.9(2) . . ? C3 Pd1 C30A 153.3(6) . . ? C3 Pd1 C31A 161.1(5) . . ? C29 Pd1 C17 172.71(19) . . ? C29 Pd1 C31 66.9(2) . . ? C29 Pd1 C30 37.1(3) . . ? C29 Pd1 C31A 70.3(5) . . ? C31 Pd1 C17 120.2(2) . . ? C30 Pd1 C17 149.9(2) . . ? C30 Pd1 C31 36.7(3) . . ? C30A Pd1 C17 144.2(7) . . ? C30A Pd1 C29 42.9(7) . . ? C30A Pd1 C31A 35.4(4) . . ? C31A Pd1 C17 116.7(5) . . ? C3 N1 C17 111.7(3) . . ? C3 N1 C2 125.5(4) . . ? C17 N1 C2 122.5(3) . . ? C3 N2 C5 120.2(4) . . ? C3 N2 C4 121.9(3) . . ? C5 N2 C4 117.9(3) . . ? N1 C3 Pd1 102.4(3) . . ? N2 C3 Pd1 137.7(3) . . ? N2 C3 N1 119.8(4) . . ? C5 C10 C14 123.3(4) . . ? C9 C10 C5 116.4(5) . . ? C9 C10 C14 120.3(5) . . ? C10 C5 N2 118.2(4) . . ? C6 C5 N2 118.2(4) . . ? C6 C5 C10 123.5(4) . . ? N1 C17 Pd1 84.3(2) . . ? C22 C17 Pd1 92.1(3) . . ? C22 C17 N1 119.2(4) . . ? C18 C17 Pd1 96.0(3) . . ? C18 C17 N1 119.4(4) . . ? C18 C17 C22 121.2(4) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C22 C21 C20 121.3(5) . . ? N2 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? N2 C4 C1 109.8(4) . . ? H4A C4 H4B 108.2 . . ? C1 C4 H4A 109.7 . . ? C1 C4 H4B 109.7 . . ? C21 C20 H20 119.9 . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C17 C22 C26 122.1(4) . . ? C21 C22 C17 118.0(4) . . ? C21 C22 C26 119.9(4) . . ? C17 C18 C23 122.1(4) . . ? C19 C18 C17 117.8(4) . . ? C19 C18 C23 120.1(4) . . ? C5 C6 C7 116.3(5) . . ? C5 C6 C11 122.8(4) . . ? C7 C6 C11 120.9(5) . . ? C18 C23 H23 108.0 . . ? C18 C23 C24 110.8(4) . . ? C25 C23 C18 112.0(4) . . ? C25 C23 H23 108.0 . . ? C25 C23 C24 109.9(4) . . ? C24 C23 H23 108.0 . . ? C10 C9 H9 118.9 . . ? C8 C9 C10 122.2(6) . . ? C8 C9 H9 118.9 . . ? C20 C19 C18 121.5(5) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? N1 C2 H2A 110.1 . . ? N1 C2 H2B 110.1 . . ? N1 C2 C1 108.1(3) . . ? H2A C2 H2B 108.4 . . ? C1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? C4 C1 C2 109.6(4) . . ? C4 C1 H1A 109.8 . . ? C4 C1 H1B 109.8 . . ? C2 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C6 C7 H7 119.0 . . ? C8 C7 C6 122.0(5) . . ? C8 C7 H7 119.0 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C9 C8 H8 120.2 . . ? C7 C8 C9 119.6(5) . . ? C7 C8 H8 120.2 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? C22 C26 C27 111.2(4) . . ? C22 C26 H26 107.8 . . ? C22 C26 C28 112.3(4) . . ? C27 C26 H26 107.8 . . ? C28 C26 C27 109.6(4) . . ? C28 C26 H26 107.8 . . ? C10 C14 H14 107.3 . . ? C10 C14 C16 111.4(5) . . ? C16 C14 H14 107.3 . . ? C15 C14 C10 112.1(5) . . ? C15 C14 H14 107.3 . . ? C15 C14 C16 111.0(5) . . ? C6 C11 H11 108.2 . . ? C6 C11 C12 111.3(5) . . ? C12 C11 H11 108.2 . . ? C13 C11 C6 110.4(6) . . ? C13 C11 H11 108.2 . . ? C13 C11 C12 110.4(5) . . ? Cl2S C1S H1S 111.0 . . ? Cl2S C1S H1SA 102.7 . . ? Cl2S C1S Cl3S 107.4(4) . . ? Cl2S C1S Cl1 112.7(4) . . ? Cl1S C1S H1S 111.0 . . ? Cl1S C1S H1SA 102.7 . . ? Cl1S C1S Cl2S 110.6(4) . . ? Cl1S C1S Cl3S 105.8(4) . . ? Cl1S C1S Cl1 122.5(5) . . ? Cl3S C1S H1S 111.0 . . ? Cl1 C1S H1SA 102.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Pd1 C29 H29A 116.2 . . ? Pd1 C29 H29B 116.2 . . ? H29A C29 H29B 113.2 . . ? C30 C29 Pd1 73.1(4) . . ? C30 C29 H29A 116.2 . . ? C30 C29 H29B 116.2 . . ? C30A C29 Pd1 68.5(8) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Pd1 C31 H31 112.2 . . ? C30 C31 Pd1 67.4(4) . . ? C30 C31 H31 112.2 . . ? C30 C31 C32 126.9(7) . . ? C32 C31 Pd1 118.5(4) . . ? C32 C31 H31 112.2 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Pd1 C30 H30 118.2 . . ? C29 C30 Pd1 69.8(4) . . ? C29 C30 C31 122.7(8) . . ? C29 C30 H30 118.2 . . ? C31 C30 Pd1 75.9(4) . . ? C31 C30 H30 118.2 . . ? F1 B1 F2 106.8(6) . . ? F1 B1 F3 115.2(5) . . ? F1 B1 F4 114.3(5) . . ? F1 B1 F3A 97.6(8) . . ? F2 B1 F3 103.0(5) . . ? F4 B1 F2 108.1(5) . . ? F4 B1 F3 108.5(6) . . ? F2A B1 F1 126.8(9) . . ? F2A B1 F3A 108.7(6) . . ? F2A B1 F4A 111.2(7) . . ? F4A B1 F1 107.4(8) . . ? F4A B1 F3A 101.7(11) . . ? C33 C32 C31 119.2(5) . . ? C33 C32 C37 120.0 . . ? C37 C32 C31 120.8(5) . . ? C31A C32 C33A 96.0(10) . . ? C37A C32 C31A 149.2(11) . . ? C37A C32 C33A 114.0(9) . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 H35 120.0 . . ? C34 C35 C36 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C32 C37 H37 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37 120.0 . . ? Pd1 C30A H30A 117.7 . . ? C29 C30A Pd1 68.6(9) . . ? C29 C30A H30A 117.7 . . ? C31A C30A Pd1 83.1(13) . . ? C31A C30A C29 125(2) . . ? C31A C30A H30A 117.7 . . ? Pd1 C31A H31A 119.3 . . ? C32 C31A Pd1 113.7(11) . . ? C32 C31A H31A 119.3 . . ? C30A C31A Pd1 61.4(12) . . ? C30A C31A C32 110.4(18) . . ? C30A C31A H31A 119.3 . . ? C32 C33A H33A 118.4 . . ? C34A C33A C32 123.2(12) . . ? C34A C33A H33A 118.4 . . ? C33A C34A H34A 119.3 . . ? C33A C34A C35A 121.5(14) . . ? C35A C34A H34A 119.3 . . ? C34A C35A H35A 120.3 . . ? C34A C35A C36A 119.4(13) . . ? C36A C35A H35A 120.3 . . ? C35A C36A H36A 120.8 . . ? C37A C36A C35A 118.4(12) . . ? C37A C36A H36A 120.8 . . ? C32 C37A C36A 123.3(13) . . ? C32 C37A H37A 118.4 . . ? C36A C37A H37A 118.4 . . ? _shelx_res_file ; TITL a_a.res in P2(1)/n a.res created by SHELXL-2018/3 at 05:32:30 on 01-Jul-2019 REM Old TITL a in Pn REM SHELXT solution in P2(1)/n REM R1 0.216, Rweak 0.027, Alpha 0.068, Orientation as input REM Formula found by SHELXT: C39 B2 N4 F2 Pd CELL 0.71073 12.2879 12.5324 25.74 90 101.171 90 ZERR 4 0.0006 0.0007 0.0014 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B Cl F N Pd UNIT 152 199.54 4 12 16 8 4 SADI 0.005 Cl1 C1S Cl3S C1S SADI 0.005 C31A C30A C31 C30 SADI 0.01 F4A F2A F4 F2 F3 F2 F3A F2A SADI 0.005 B1 F4A B1 F4 B1 F3 B1 F3A B1 F2A B1 F2 B1 F1 SIMU 0.005 0.005 1.7 Cl1 Cl3S SIMU 0.005 0.005 1.7 F4A F2 F2A F3 F3A F4 SIMU 0.005 0.005 1.7 C32 C33 C33A C34 C34A C35A C35 C36 C36A C37 C37A RIGU Cl3S Cl1 L.S. 30 PLAN 20 TEMP -153 BOND $H fmap 2 acta OMIT 1 0 1 REM REM REM WGHT 0.030100 28.336500 FVAR 0.35477 0.66075 0.77518 0.69682 0.50753 PD1 7 0.660189 0.697987 0.358398 11.00000 0.02562 0.03902 = 0.02591 -0.00907 0.01320 -0.01198 N1 6 0.611900 0.733010 0.453726 11.00000 0.01982 0.02106 = 0.02149 -0.00167 0.00914 -0.00275 N2 6 0.744348 0.861667 0.450685 11.00000 0.01993 0.01930 = 0.02498 -0.00454 0.00967 -0.00271 C3 1 0.683330 0.780426 0.428240 11.00000 0.01959 0.01631 = 0.02370 -0.00107 0.00988 -0.00044 F1 5 0.636913 0.767043 0.633716 11.00000 0.11555 0.07356 = 0.06081 -0.00230 0.02099 -0.04459 C10 1 0.781501 0.999247 0.388762 11.00000 0.03203 0.03599 = 0.02620 -0.00246 0.00821 -0.00983 C5 1 0.821289 0.914728 0.422949 11.00000 0.02274 0.02579 = 0.02930 -0.00635 0.01181 -0.01002 C17 1 0.549313 0.651022 0.421966 11.00000 0.01410 0.02313 = 0.02379 0.00120 0.00932 -0.00129 C21 1 0.386596 0.597030 0.359112 11.00000 0.01910 0.04456 = 0.03348 0.00064 0.00527 -0.00825 AFIX 43 H21 2 0.320073 0.613910 0.334960 11.00000 -1.20000 AFIX 0 C4 1 0.735192 0.902603 0.503782 11.00000 0.02777 0.02786 = 0.02636 -0.00773 0.01072 -0.00575 AFIX 23 H4A 2 0.752447 0.979824 0.505998 11.00000 -1.20000 H4B 2 0.789290 0.865417 0.531358 11.00000 -1.20000 AFIX 0 C20 1 0.419412 0.490697 0.366318 11.00000 0.02745 0.03269 = 0.03213 -0.00793 0.00976 -0.01266 AFIX 43 H20 2 0.373861 0.435827 0.348200 11.00000 -1.20000 AFIX 0 C22 1 0.449267 0.678865 0.386560 11.00000 0.02047 0.02793 = 0.02815 0.00152 0.00760 -0.00102 C18 1 0.585578 0.543254 0.428327 11.00000 0.02007 0.02090 = 0.02582 0.00010 0.01093 -0.00048 C6 1 0.932129 0.881271 0.433233 11.00000 0.02348 0.03399 = 0.04275 -0.01122 0.01473 -0.00570 C23 1 0.693511 0.512059 0.465007 11.00000 0.02141 0.02270 = 0.03106 0.00223 0.00774 0.00079 AFIX 13 H23 2 0.725183 0.577437 0.484552 11.00000 -1.20000 AFIX 0 C9 1 0.859429 1.051194 0.364652 11.00000 0.05226 0.04857 = 0.02989 -0.00135 0.01365 -0.02414 AFIX 43 H9 2 0.835458 1.108032 0.340749 11.00000 -1.20000 AFIX 0 C19 1 0.518125 0.464911 0.399780 11.00000 0.03075 0.02556 = 0.03285 -0.00468 0.01369 -0.00435 AFIX 43 H19 2 0.540607 0.392331 0.403451 11.00000 -1.20000 AFIX 0 C2 1 0.588292 0.766342 0.505371 11.00000 0.02985 0.02252 = 0.02528 -0.00416 0.01474 -0.00297 AFIX 23 H2A 2 0.632767 0.723355 0.534130 11.00000 -1.20000 H2B 2 0.508772 0.755442 0.506023 11.00000 -1.20000 AFIX 0 C1 1 0.618083 0.884180 0.513300 11.00000 0.03019 0.02084 = 0.02941 -0.00479 0.01453 0.00129 AFIX 23 H1A 2 0.564794 0.927949 0.488315 11.00000 -1.20000 H1B 2 0.613663 0.905966 0.549803 11.00000 -1.20000 AFIX 0 C7 1 1.005141 0.938753 0.407799 11.00000 0.03160 0.05003 = 0.05313 -0.01486 0.02581 -0.01217 AFIX 43 H7 2 1.081180 0.918942 0.413889 11.00000 -1.20000 AFIX 0 C25 1 0.675358 0.429473 0.505443 11.00000 0.03061 0.03962 = 0.03672 0.01197 0.01062 0.00280 AFIX 137 H25A 2 0.618790 0.455148 0.524531 11.00000 -1.50000 H25B 2 0.745040 0.417396 0.530595 11.00000 -1.50000 H25C 2 0.650498 0.362444 0.487367 11.00000 -1.50000 AFIX 0 C8 1 0.969796 1.022680 0.374416 11.00000 0.04572 0.05518 = 0.04418 -0.01195 0.02861 -0.02644 AFIX 43 H8 2 1.021123 1.060778 0.358181 11.00000 -1.20000 AFIX 0 C27 1 0.396222 0.827898 0.320830 11.00000 0.03734 0.04678 = 0.04539 0.01402 0.00858 0.00585 AFIX 137 H27A 2 0.468248 0.823699 0.309956 11.00000 -1.50000 H27B 2 0.368779 0.901454 0.316947 11.00000 -1.50000 H27C 2 0.343297 0.780572 0.298494 11.00000 -1.50000 AFIX 0 C26 1 0.409306 0.793346 0.379008 11.00000 0.02196 0.02924 = 0.03685 0.00509 0.00527 -0.00007 AFIX 13 H26 2 0.466825 0.840088 0.400630 11.00000 -1.20000 AFIX 0 C14 1 0.660872 1.035746 0.377953 11.00000 0.03146 0.04586 = 0.03547 0.01429 0.00069 -0.00856 AFIX 13 H14 2 0.617817 0.982475 0.394708 11.00000 -1.20000 AFIX 0 C11 1 0.972489 0.786554 0.468233 11.00000 0.02366 0.02937 = 0.06141 -0.00499 0.01415 0.00247 AFIX 13 H11 2 0.913162 0.766659 0.488113 11.00000 -1.20000 AFIX 0 C1S 1 0.931424 0.611304 0.650862 11.00000 0.03484 0.05683 = 0.04486 -0.00993 -0.00061 -0.00804 PART 1 AFIX 13 H1S 2 0.878847 0.659227 0.664935 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H1SA 2 0.886983 0.674236 0.658468 -21.00000 -1.20000 AFIX 0 PART 0 C24 1 0.778082 0.470532 0.433156 11.00000 0.02815 0.04829 = 0.04533 0.00553 0.01550 0.00839 AFIX 137 H24A 2 0.750692 0.404013 0.415258 11.00000 -1.50000 H24B 2 0.849020 0.457172 0.457138 11.00000 -1.50000 H24C 2 0.788564 0.523880 0.406725 11.00000 -1.50000 AFIX 0 C28 1 0.299811 0.811214 0.397961 11.00000 0.03432 0.04471 = 0.05886 0.01081 0.02189 0.01032 AFIX 137 H28A 2 0.243532 0.761815 0.379477 11.00000 -1.50000 H28B 2 0.274853 0.884826 0.390324 11.00000 -1.50000 H28C 2 0.311090 0.798418 0.436191 11.00000 -1.50000 AFIX 0 C29 1 0.764791 0.754711 0.309512 11.00000 0.04590 0.06377 = 0.03328 -0.01116 0.02250 -0.02575 AFIX 23 H29A 2 0.736122 0.814902 0.285880 11.00000 -1.20000 H29B 2 0.844092 0.762407 0.326113 11.00000 -1.20000 AFIX 0 C16 1 0.611652 1.036821 0.318304 11.00000 0.05823 0.04699 = 0.04080 0.00905 -0.00795 -0.00628 AFIX 137 H16A 2 0.648462 1.092057 0.300994 11.00000 -1.50000 H16B 2 0.532021 1.052053 0.312855 11.00000 -1.50000 H16C 2 0.623099 0.967039 0.303039 11.00000 -1.50000 AFIX 0 C12 1 1.077167 0.813759 0.508327 11.00000 0.05260 0.03753 = 0.05751 -0.01607 0.00642 -0.00274 AFIX 137 H12A 2 1.138676 0.825506 0.489788 11.00000 -1.50000 H12B 2 1.095536 0.754618 0.533401 11.00000 -1.50000 H12C 2 1.064617 0.878653 0.527580 11.00000 -1.50000 AFIX 0 C15 1 0.646738 1.142946 0.402717 11.00000 0.03999 0.07187 = 0.04940 -0.00909 0.00312 0.00651 AFIX 137 H15A 2 0.666890 1.137004 0.441352 11.00000 -1.50000 H15B 2 0.569264 1.165846 0.392601 11.00000 -1.50000 H15C 2 0.694897 1.195499 0.390255 11.00000 -1.50000 AFIX 0 PART 1 C31 1 0.621516 0.629499 0.276536 31.00000 0.03024 0.03612 = 0.02222 -0.00083 0.00915 -0.00809 AFIX 13 H31 2 0.580134 0.680957 0.250214 21.00000 -1.20000 AFIX 0 PART 0 C13 1 0.992980 0.691922 0.434896 11.00000 0.04914 0.04446 = 0.10232 -0.03440 -0.01228 0.00325 AFIX 137 H13A 2 0.925851 0.676933 0.408491 11.00000 -1.50000 H13B 2 1.011998 0.629398 0.457714 11.00000 -1.50000 H13C 2 1.054360 0.708152 0.416893 11.00000 -1.50000 AFIX 0 PART 1 C30 1 0.731796 0.656848 0.292031 31.00000 0.02551 0.04945 = 0.02991 -0.00846 0.01692 -0.00690 AFIX 13 H30 2 0.788329 0.598482 0.296391 31.00000 -1.20000 AFIX 0 PART 0 B1 3 0.711927 0.832933 0.663645 11.00000 0.04070 0.04762 = 0.05098 0.00340 0.01065 0.00351 CL2S 4 1.068491 0.657161 0.669431 11.00000 0.04121 0.07502 = 0.07833 -0.02561 0.00718 -0.01553 CL1S 4 0.894367 0.599504 0.582266 11.00000 0.08882 0.07968 = 0.04874 -0.01906 -0.01775 0.01615 PART 1 F2 5 0.792984 0.769261 0.691815 41.00000 0.10570 0.08615 = 0.08483 -0.00360 -0.00776 0.03716 F3 5 0.673347 0.887733 0.702480 41.00000 0.08467 0.07544 = 0.09276 -0.02528 0.03672 0.00098 F4 5 0.760981 0.903589 0.635182 41.00000 0.08382 0.08963 = 0.07580 0.01512 0.01409 -0.03236 PART 0 AFIX 66 C32 1 0.574539 0.519594 0.269336 11.00000 0.04207 0.04579 = 0.02665 -0.00911 0.01377 -0.01156 PART 1 C33 1 0.642043 0.433084 0.287518 51.00000 0.04345 0.04116 = 0.03016 -0.01218 0.01248 -0.01306 AFIX 43 H33 2 0.717514 0.444286 0.303612 51.00000 -1.20000 AFIX 65 C34 1 0.599122 0.330182 0.282150 51.00000 0.04591 0.04445 = 0.03415 -0.00854 0.01321 -0.01090 AFIX 43 H34 2 0.645258 0.271057 0.294576 51.00000 -1.20000 AFIX 65 C35 1 0.488697 0.313790 0.258602 51.00000 0.04841 0.04525 = 0.03638 -0.00837 0.01214 -0.01268 AFIX 43 H35 2 0.459363 0.243461 0.254933 51.00000 -1.20000 AFIX 65 C36 1 0.421192 0.400299 0.240420 51.00000 0.05002 0.04883 = 0.03601 -0.00618 0.00983 -0.01180 AFIX 43 H36 2 0.345721 0.389096 0.224326 51.00000 -1.20000 AFIX 65 C37 1 0.464111 0.503201 0.245787 51.00000 0.04779 0.04877 = 0.03144 -0.00483 0.01009 -0.00951 AFIX 43 H37 2 0.417974 0.562326 0.233361 51.00000 -1.20000 AFIX 0 CL3S 4 0.927120 0.479533 0.676152 21.00000 0.07751 0.07274 = 0.07379 0.01217 0.01042 -0.01807 PART 0 PART 2 CL1 4 0.897629 0.513175 0.694474 -21.00000 0.06531 0.07931 = 0.06722 0.00970 0.00571 -0.02079 C30A 1 0.681800 0.673430 0.280771 -31.00000 0.01172 0.05458 = 0.02392 -0.00381 0.01019 -0.00217 AFIX 13 H30A 2 0.622462 0.700034 0.251424 -31.00000 -1.20000 AFIX 0 C31A 1 0.678759 0.567310 0.294601 -31.00000 0.02760 0.03769 = 0.01512 -0.00751 0.00402 0.00032 AFIX 13 H31A 2 0.748280 0.523938 0.299224 -31.00000 -1.20000 AFIX 0 F2A 5 0.743537 0.831875 0.716847 -41.00000 0.09993 0.08670 = 0.09035 -0.00554 0.00819 0.00940 F3A 5 0.659063 0.926702 0.648867 -41.00000 0.08825 0.07705 = 0.08729 -0.01201 0.02134 -0.00864 F4A 5 0.800893 0.839676 0.639771 -41.00000 0.08477 0.08095 = 0.08167 0.00693 0.01475 0.00019 C33A 1 0.608463 0.407888 0.282064 -51.00000 0.04440 0.04829 = 0.03239 -0.01199 0.01005 -0.00566 AFIX 43 H33A 2 0.682107 0.394653 0.300323 -51.00000 -1.20000 AFIX 0 C34A 1 0.542776 0.327311 0.269554 -51.00000 0.05115 0.04590 = 0.03635 -0.00802 0.00948 -0.00345 AFIX 43 H34A 2 0.570389 0.257192 0.277528 -51.00000 -1.20000 AFIX 0 C35A 1 0.435519 0.340673 0.245343 -51.00000 0.04978 0.04582 = 0.03525 -0.00653 0.01138 -0.00967 AFIX 43 H35A 2 0.388830 0.280504 0.235948 -51.00000 -1.20000 AFIX 0 C36A 1 0.393520 0.445515 0.234134 -51.00000 0.04365 0.04800 = 0.03279 -0.00237 0.00871 -0.00808 AFIX 43 H36A 2 0.318007 0.456824 0.218144 -51.00000 -1.20000 AFIX 0 C37A 1 0.465578 0.531202 0.247127 -51.00000 0.04677 0.04699 = 0.03029 -0.00378 0.01176 -0.00829 AFIX 43 H37A 2 0.437161 0.601331 0.240117 -51.00000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in P2(1)/n REM wR2 = 0.1854, GooF = S = 1.105, Restrained GooF = 1.127 for all data REM R1 = 0.0843 for 9521 Fo > 4sig(Fo) and 0.1039 for all 11877 data REM 541 parameters refined using 197 restraints END WGHT 0.0306 21.8608 REM Highest difference peak 1.823, deepest hole -2.107, 1-sigma level 0.122 Q1 1 0.7191 0.7746 0.3563 11.00000 0.05 1.82 Q2 1 0.8440 0.8065 0.6826 11.00000 0.05 1.37 Q3 1 0.7005 0.8604 0.7184 11.00000 0.05 1.35 Q4 1 0.7619 0.7411 0.6983 11.00000 0.05 1.34 Q5 1 0.7861 0.8393 0.6230 11.00000 0.05 1.33 Q6 1 0.6612 0.7590 0.3298 11.00000 0.05 1.15 Q7 1 0.6730 0.6431 0.3610 11.00000 0.05 1.10 Q8 1 0.4978 0.7567 0.4164 11.00000 0.05 0.92 Q9 1 0.7236 0.9387 0.6389 11.00000 0.05 0.90 Q10 1 0.5854 0.3645 0.2829 11.00000 0.05 0.71 Q11 1 0.6432 0.9008 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6 -8 22 56.69 15.50 -6 -8 -22 45.10 17.40 -6 8 -22 98.39 21.60 -6 8 -22 56.19 16.50 6 8 22 44.80 18.50 7 -8 22 -0.40 11.00 -7 -8 -22 8.20 12.90 7 -8 22 3.40 13.90 -7 8 -22 17.30 13.90 7 8 22 -11.80 13.70 -7 8 -22 23.00 15.90 8 -8 22 -17.80 13.40 -8 -8 -22 -1.60 12.90 8 -8 22 8.50 13.30 8 8 22 18.80 18.60 -8 8 -22 2.10 13.20 -8 8 -22 -7.80 14.90 9 -8 22 12.30 16.60 -9 -8 -22 13.40 14.90 9 -8 22 36.10 15.60 9 8 22 29.90 18.60 -9 8 -22 77.19 20.70 -12 -9 22 5.60 10.60 12 -9 -22 36.40 21.30 12 9 -22 25.80 14.40 -12 9 22 31.10 18.10 -12 9 22 4.00 13.80 12 9 -22 0.60 15.60 -11 -9 22 9.30 11.00 11 -9 -22 15.90 19.70 -11 -9 22 28.40 13.00 11 9 -22 41.10 16.40 -11 9 22 24.20 18.30 -11 9 22 22.40 13.50 11 9 -22 6.90 12.80 -10 -9 22 58.69 14.20 -10 -9 22 79.99 16.50 10 -9 -22 60.59 22.70 10 9 -22 84.99 24.90 10 9 -22 60.39 16.60 -10 9 22 43.70 15.30 -10 9 22 67.39 19.50 9 -9 -22 6.50 17.20 -9 -9 22 -0.70 9.80 -9 -9 22 9.80 11.10 -9 9 22 16.30 15.80 9 9 -22 -0.30 12.30 -9 9 22 11.80 11.90 -8 -9 22 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18.30 13.70 7 2 -28 29.30 15.60 -7 2 28 43.50 11.70 7 2 -28 36.60 16.80 -7 2 28 40.90 15.40 6 -2 -28 175.98 23.90 -6 -2 28 154.18 20.70 6 -2 -28 170.48 23.70 -6 -2 28 185.48 19.80 -6 2 28 153.78 20.80 6 2 -28 165.28 22.10 6 2 -28 159.58 21.70 -6 2 28 192.58 19.30 5 -2 -28 81.39 18.70 5 -2 -28 100.49 19.20 -5 -2 28 95.69 16.20 -5 -2 28 63.49 16.10 -5 2 28 80.89 15.50 -5 2 28 97.99 17.80 5 2 -28 94.09 19.30 5 2 -28 99.79 17.70 -4 -2 28 87.49 15.50 4 -2 -28 46.40 16.70 -4 -2 28 104.09 18.50 4 -2 -28 82.49 18.50 4 2 -28 82.49 18.10 -4 2 28 87.49 17.20 -4 2 28 112.19 17.30 4 2 -28 109.09 18.10 3 -2 -28 -2.40 12.20 -3 -2 28 -4.10 9.80 -3 -2 28 -14.10 9.80 3 -2 -28 9.00 12.80 -3 2 28 -1.60 9.60 -3 2 28 3.40 11.30 3 2 -28 -1.30 11.90 3 2 -28 22.20 14.70 -2 -2 28 -8.80 10.80 -2 -2 28 17.80 12.10 2 -2 -28 1.80 12.40 2 -2 -28 8.70 12.60 2 2 -28 -5.90 11.00 -2 2 28 3.10 10.80 -2 2 28 -4.80 12.70 2 2 -28 -4.70 11.20 -1 -2 28 65.19 15.30 1 -2 -28 57.09 15.70 -1 -2 28 49.50 15.00 1 -2 -28 85.99 17.20 -1 2 28 72.09 16.10 -1 2 28 97.89 17.70 1 2 -28 87.59 16.40 1 2 -28 71.29 16.40 0 -2 -28 120.59 19.20 0 -2 -28 122.09 19.90 0 -2 28 89.19 17.90 0 -2 28 121.99 18.40 0 2 28 102.99 16.60 0 2 -28 72.29 17.20 0 2 28 140.69 21.90 1 -2 28 3.50 11.70 -1 -2 -28 9.90 12.30 1 -2 28 -4.70 10.10 -1 -2 -28 0.00 12.90 -1 2 -28 14.50 12.60 1 2 28 14.70 10.60 1 2 28 1.50 14.30 2 -2 28 36.90 15.80 -2 -2 -28 11.90 14.20 -2 -2 -28 4.00 12.30 2 -2 28 20.70 11.40 2 2 28 9.90 10.90 -2 2 -28 29.60 13.70 2 2 28 42.60 15.80 3 -2 28 13.80 10.60 3 -2 28 26.20 14.30 -3 -2 -28 10.50 12.20 -3 -2 -28 -6.20 13.90 3 2 28 -11.60 14.90 3 2 28 11.40 10.10 -3 2 -28 11.50 15.00 -4 -2 -28 68.89 17.20 4 -2 28 68.99 14.30 4 -2 28 39.70 16.30 -4 -2 -28 74.89 17.80 -4 2 -28 63.09 19.40 4 2 28 107.89 22.80 -5 -2 -28 16.40 13.80 5 -2 28 28.60 15.10 -5 -2 -28 6.50 12.80 -5 2 -28 3.00 13.30 -5 2 -28 6.60 11.70 5 2 28 3.10 17.10 -6 -2 -28 112.89 18.60 -6 -2 -28 108.09 20.80 6 -2 28 69.79 19.40 -6 2 -28 89.19 20.50 6 2 28 95.89 23.30 -7 -2 -28 12.70 16.90 7 -2 28 4.00 16.10 -7 2 -28 14.60 17.40 7 2 28 -5.60 16.30 -8 -2 -28 2.20 15.10 8 -2 28 -25.70 13.70 8 2 28 -6.70 17.20 -8 2 -28 -35.30 13.50 13 -3 -28 107.59 25.50 -13 -3 28 134.09 25.70 -13 -3 28 131.09 23.70 13 3 -28 114.59 26.20 -13 3 28 132.79 24.90 -13 3 28 159.88 25.00 12 -3 -28 12.90 18.70 -12 -3 28 -5.20 13.50 -12 -3 28 -2.30 14.30 -12 3 28 -16.50 13.10 -12 3 28 -2.00 14.70 12 3 -28 35.00 18.80 11 -3 -28 97.49 22.90 -11 -3 28 141.69 24.00 -11 3 28 73.79 20.30 11 3 -28 122.39 24.30 11 3 -28 125.89 25.40 -11 3 28 105.69 23.60 10 -3 -28 18.60 17.40 -10 -3 28 19.30 15.20 -10 3 28 7.60 13.70 -10 3 28 -9.20 11.30 10 3 -28 25.90 17.50 10 3 -28 5.20 14.60 -9 -3 28 255.87 27.40 9 -3 -28 211.08 30.10 9 -3 -28 178.88 24.60 -9 3 28 196.08 24.70 9 3 -28 231.58 28.00 9 3 -28 234.68 27.30 8 -3 -28 151.08 24.50 8 -3 -28 130.29 21.30 -8 -3 28 175.38 23.70 -8 -3 28 203.28 20.30 8 3 -28 209.68 27.30 8 3 -28 234.48 26.40 -8 3 28 182.78 24.10 -7 -3 28 107.69 19.20 7 -3 -28 151.38 23.00 7 -3 -28 109.89 20.70 -7 -3 28 102.59 16.20 7 3 -28 108.39 19.40 7 3 -28 105.69 21.30 -7 3 28 139.99 21.50 6 -3 -28 69.79 18.00 -6 -3 28 88.59 15.20 6 -3 -28 107.49 20.60 -6 -3 28 89.89 17.30 -6 3 28 50.69 16.00 6 3 -28 66.59 17.10 6 3 -28 95.89 19.60 -6 3 28 117.79 16.10 5 -3 -28 -4.20 13.40 -5 -3 28 -16.30 10.50 5 -3 -28 -2.10 12.70 -5 -3 28 1.60 9.60 5 3 -28 -21.80 11.40 5 3 -28 -8.90 12.60 -5 3 28 18.80 13.70 -5 3 28 4.50 11.40 -4 -3 28 66.49 16.00 4 -3 -28 98.49 17.70 4 -3 -28 60.99 16.90 -4 -3 28 87.49 16.40 4 3 -28 105.69 17.30 -4 3 28 140.29 19.60 -4 3 28 93.99 16.50 4 3 -28 66.49 18.50 3 -3 -28 88.49 18.30 -3 -3 28 112.99 18.40 3 -3 -28 119.99 18.90 -3 -3 28 98.59 17.70 -3 3 28 102.49 17.30 3 3 -28 92.19 20.10 -3 3 28 88.99 17.00 3 3 -28 131.89 19.50 2 -3 -28 196.58 23.10 -2 -3 28 147.39 20.10 -2 -3 28 194.68 23.20 2 -3 -28 161.38 22.20 -2 3 28 190.78 21.50 -2 3 28 164.78 22.20 2 3 -28 116.39 20.00 -1 -3 28 120.49 20.40 1 -3 -28 120.49 18.60 -1 -3 28 201.78 22.10 1 -3 -28 120.89 19.20 -1 3 28 133.69 21.50 -1 3 28 122.59 18.60 1 3 -28 153.68 22.50 0 -3 28 -10.80 9.80 0 -3 -28 -4.90 12.50 0 -3 -28 -10.10 11.40 0 -3 28 6.20 11.20 0 3 -28 -20.50 12.10 0 3 28 13.50 12.70 0 3 28 13.30 11.70 -1 -3 -28 -7.70 12.40 1 -3 28 0.30 11.40 -1 -3 -28 12.60 13.70 1 -3 28 -0.80 12.50 1 3 28 5.50 16.20 1 3 28 24.60 12.00 -1 3 -28 6.00 12.00 -2 -3 -28 71.19 17.90 2 -3 28 104.39 17.50 -2 -3 -28 39.00 15.00 2 -3 28 48.70 16.10 2 3 28 84.09 14.50 2 3 28 72.69 20.00 -2 3 -28 46.60 15.60 3 -3 28 77.39 14.90 -3 -3 -28 52.69 16.80 -3 -3 -28 71.29 15.90 3 -3 28 96.99 20.90 3 3 28 74.59 13.90 -4 -3 -28 -3.70 13.50 4 -3 28 -4.80 13.90 -4 -3 -28 12.70 12.70 4 3 28 21.50 15.00 -4 3 -28 5.60 11.50 -4 3 -28 -4.00 14.20 -5 -3 -28 -5.50 11.70 -5 -3 -28 -14.70 12.20 5 -3 28 47.50 18.00 -5 3 -28 -15.70 13.80 5 3 28 21.30 17.70 -5 3 -28 -1.30 11.40 6 -3 28 16.00 16.20 -6 -3 -28 -3.30 12.80 -6 -3 -28 3.30 14.00 6 3 28 0.10 17.10 -6 3 -28 10.80 16.20 -7 -3 -28 23.60 14.50 7 -3 28 -12.50 12.00 -7 -3 -28 -6.00 14.90 -7 3 -28 15.80 17.30 7 3 28 14.00 18.00 -8 -3 -28 17.70 14.50 8 -3 28 -4.40 13.60 -8 -3 -28 3.00 14.10 8 3 28 21.80 18.90 -8 3 -28 -31.30 13.60 -13 -4 28 2.50 15.40 13 -4 -28 -9.20 19.10 -13 -4 28 -16.60 13.90 -13 4 28 4.90 14.80 13 4 -28 -1.90 17.40 -13 4 28 -34.60 12.10 12 -4 -28 47.10 19.80 -12 -4 28 22.90 15.90 -12 4 28 -9.20 14.60 12 4 -28 -15.30 16.40 12 4 -28 34.30 19.80 -12 4 28 6.30 13.30 11 -4 -28 218.08 31.60 -11 -4 28 264.37 30.30 11 4 -28 201.98 29.30 -11 4 28 223.28 29.00 -11 4 28 278.27 30.10 11 4 -28 207.88 28.20 10 -4 -28 10.00 18.00 -10 4 28 12.50 15.20 10 4 -28 6.80 16.80 -10 4 28 7.10 14.20 10 4 -28 8.50 15.30 -9 -4 28 155.18 24.10 9 -4 -28 125.79 24.40 9 -4 -28 164.38 24.40 9 4 -28 132.29 23.90 9 4 -28 163.38 24.20 -9 4 28 171.48 24.30 -8 -4 28 13.10 9.50 8 -4 -28 -1.40 14.60 -8 -4 28 9.80 13.70 8 -4 -28 -4.20 14.20 8 4 -28 1.30 14.00 -8 4 28 -4.30 12.70 8 4 -28 10.80 15.80 -7 -4 28 72.79 17.50 7 -4 -28 75.19 17.00 7 -4 -28 57.09 18.70 -7 -4 28 70.99 14.70 -7 4 28 63.99 17.50 7 4 -28 59.69 18.40 7 4 -28 69.39 16.80 -6 -4 28 50.29 14.00 6 -4 -28 70.99 19.20 -6 -4 28 53.39 14.50 6 -4 -28 76.29 18.10 6 4 -28 48.50 15.40 -6 4 28 67.89 16.10 -6 4 28 78.89 14.70 6 4 -28 87.09 16.90 5 -4 -28 131.89 21.80 5 -4 -28 206.48 25.00 -5 -4 28 130.09 18.40 -5 -4 28 164.58 21.70 5 4 -28 180.38 24.40 -5 4 28 208.08 21.40 -5 4 28 160.28 21.60 5 4 -28 203.18 24.60 -4 -4 28 4.80 11.30 -4 -4 28 -4.30 10.80 4 -4 -28 12.80 12.00 4 -4 -28 5.80 14.10 -4 4 28 30.00 14.20 -4 4 28 11.00 12.30 4 4 -28 11.60 12.40 -3 -4 28 89.89 17.90 3 -4 -28 87.39 19.20 3 -4 -28 63.09 16.00 -3 -4 28 53.89 15.30 3 4 -28 71.99 17.10 -3 4 28 81.49 16.80 -3 4 28 75.79 16.60 2 -4 -28 10.10 12.80 -2 -4 28 11.90 12.40 -2 -4 28 40.90 14.20 2 -4 -28 23.50 14.20 2 4 -28 11.50 12.80 -2 4 28 12.10 12.00 -2 4 28 -15.10 11.60 -1 -4 28 125.49 18.90 -1 -4 28 137.99 20.40 1 -4 -28 142.39 20.90 1 -4 -28 126.29 20.80 -1 4 28 123.19 21.00 1 4 -28 132.09 22.00 -1 4 28 180.38 21.40 0 -4 28 10.30 11.90 0 -4 -28 36.00 15.90 0 -4 28 35.90 13.80 0 4 -28 5.20 14.10 0 4 28 39.60 13.40 0 4 28 34.80 15.70 -1 -4 -28 409.46 30.10 1 -4 28 431.76 31.80 -1 -4 -28 401.96 30.00 1 -4 28 458.25 29.30 1 4 28 469.35 28.20 1 4 28 462.65 33.60 -1 4 -28 412.26 31.10 2 -4 28 0.90 11.90 -2 -4 -28 -2.20 12.10 -2 -4 -28 5.80 13.10 2 -4 28 44.30 14.10 2 4 28 42.40 12.40 -2 4 -28 7.40 15.30 2 4 28 -2.00 12.80 -3 -4 -28 5.70 14.30 -3 -4 -28 17.60 12.70 3 -4 28 7.80 14.80 3 -4 28 30.00 13.60 3 4 28 17.10 16.90 -3 4 -28 1.70 12.50 4 -4 28 13.60 15.70 -4 -4 -28 17.00 14.20 -4 -4 -28 51.49 16.00 -4 4 -28 12.50 15.50 4 4 28 17.10 15.30 -4 4 -28 26.10 13.80 -5 -4 -28 74.29 17.10 5 -4 28 67.19 17.70 -5 -4 -28 65.89 18.10 -5 4 -28 110.49 22.60 5 4 28 67.19 21.00 -5 4 -28 136.79 19.40 -6 -4 -28 -4.10 12.50 6 -4 28 -6.60 13.10 -6 -4 -28 -8.80 14.70 6 4 28 -14.00 16.30 -6 4 -28 -11.50 15.00 -6 4 -28 12.30 13.50 -7 -4 -28 24.20 16.30 7 -4 28 48.00 19.20 -7 4 -28 62.69 21.00 7 4 28 46.20 19.80 12 -5 -28 -2.10 18.30 -12 -5 28 25.20 13.80 -12 5 28 -1.00 15.10 12 5 -28 27.30 19.40 -12 5 28 -11.90 14.90 12 5 -28 8.20 17.50 11 -5 -28 17.80 19.10 -11 -5 28 5.40 12.80 11 5 -28 -1.80 17.00 -11 5 28 0.40 15.20 11 5 -28 -12.30 18.10 -11 5 28 -4.90 14.10 10 -5 -28 -0.50 12.40 -10 -5 28 0.50 12.40 10 -5 -28 20.30 17.40 -10 5 28 -4.60 14.00 10 5 -28 -15.50 13.60 10 5 -28 -0.10 15.50 9 -5 -28 72.99 18.80 -9 -5 28 51.89 16.90 -9 -5 28 54.09 13.50 9 -5 -28 88.09 23.00 -9 5 28 50.99 18.40 9 5 -28 47.30 17.90 8 -5 -28 3.00 16.30 -8 -5 28 35.00 11.80 8 -5 -28 20.30 15.60 -8 -5 28 34.90 14.10 8 5 -28 11.80 14.90 8 5 -28 10.30 16.00 -8 5 28 27.90 15.40 -7 -5 28 120.09 19.90 7 -5 -28 173.78 26.10 7 -5 -28 151.18 22.40 -7 -5 28 173.88 20.50 -7 5 28 149.79 21.80 7 5 -28 190.78 24.80 -6 -5 28 -5.90 9.90 6 -5 -28 19.20 16.20 6 -5 -28 4.30 13.10 -6 -5 28 1.50 11.40 6 5 -28 16.60 14.50 -6 5 28 -24.50 9.30 -6 5 28 35.70 15.00 5 -5 -28 15.10 13.40 -5 -5 28 19.70 12.40 -5 -5 28 13.70 12.50 5 -5 -28 21.60 15.50 -5 5 28 18.90 13.50 5 5 -28 26.70 14.80 -5 5 28 43.10 14.50 4 -5 -28 9.60 15.50 -4 -5 28 28.20 13.60 -4 -5 28 -1.00 9.90 4 -5 -28 15.20 13.30 4 5 -28 18.30 13.70 -4 5 28 -2.90 11.80 -4 5 28 -13.90 11.70 -3 -5 28 302.77 25.50 3 -5 -28 281.77 29.50 3 -5 -28 231.38 24.90 -3 -5 28 235.88 25.40 3 5 -28 232.38 27.00 -3 5 28 275.97 26.40 -3 5 28 314.97 25.30 2 -5 -28 -1.80 14.00 -2 -5 28 6.90 11.70 2 -5 -28 8.00 12.50 -2 -5 28 -5.40 10.60 2 5 -28 9.80 12.60 -2 5 28 -18.70 9.80 -2 5 28 -15.90 12.40 1 -5 -28 31.60 15.80 1 -5 -28 24.90 13.50 -1 -5 28 46.70 16.00 -1 -5 28 66.39 15.80 1 5 -28 44.80 16.50 -1 5 28 63.69 14.60 -1 5 28 24.10 14.20 0 -5 -28 2.00 12.90 0 -5 28 -5.40 10.60 0 -5 -28 17.60 14.30 0 -5 28 36.10 14.20 0 5 -28 28.70 15.40 0 5 28 0.80 12.70 0 5 28 3.90 10.10 1 -5 28 14.30 12.80 -1 -5 -28 12.60 12.90 -1 -5 -28 18.40 13.70 1 -5 28 2.30 13.00 1 5 28 14.20 16.70 1 5 28 13.70 10.70 -1 5 -28 20.50 13.90 -2 -5 -28 5.80 13.00 -2 -5 -28 30.50 15.10 2 -5 28 26.80 12.80 2 -5 28 4.30 11.70 2 5 28 19.50 11.40 2 5 28 27.70 15.70 -2 5 -28 20.20 15.60 -3 -5 -28 45.60 16.20 3 -5 28 10.30 14.00 -3 -5 -28 25.30 14.40 3 5 28 31.40 16.70 -3 5 -28 37.20 16.10 4 -5 28 -8.20 13.30 -4 -5 -28 0.00 12.70 -4 -5 -28 -3.60 13.30 4 5 28 23.60 17.40 -4 5 -28 1.60 13.40 -4 5 -28 1.50 12.40 -5 -5 -28 27.30 14.40 5 -5 28 35.40 17.30 -5 -5 -28 11.90 14.60 -5 5 -28 42.30 17.90 -5 5 -28 54.49 15.60 5 5 28 46.60 18.50 -6 -5 -28 -8.30 13.70 -6 -5 -28 21.80 14.30 6 -5 28 16.00 15.60 -6 5 -28 26.70 13.80 -6 5 -28 10.20 14.60 6 5 28 0.60 17.00 7 -5 28 -10.50 11.90 -7 -5 -28 2.10 13.90 -7 -5 -28 -16.80 12.50 7 5 28 -11.20 15.00 -7 5 -28 16.90 17.20 -12 -6 28 -2.80 12.90 12 -6 -28 16.00 21.00 12 6 -28 -14.80 16.40 -12 6 28 -15.30 15.50 -12 6 28 10.00 15.90 12 6 -28 17.20 18.90 11 -6 -28 118.79 25.80 -11 -6 28 123.49 20.90 11 6 -28 116.79 24.50 -11 6 28 153.88 26.00 -11 6 28 174.48 26.10 11 6 -28 170.98 25.80 10 -6 -28 0.30 17.00 -10 -6 28 10.10 13.20 10 -6 -28 0.70 15.00 10 6 -28 -19.40 14.30 -10 6 28 -9.00 13.90 10 6 -28 -5.60 14.90 9 -6 -28 2.30 17.10 -9 -6 28 12.80 13.40 9 -6 -28 -9.00 14.40 -9 -6 28 21.90 11.10 -9 6 28 2.90 14.30 9 6 -28 9.50 16.80 -8 -6 28 14.90 13.20 -8 -6 28 11.50 11.70 8 -6 -28 21.70 15.90 8 -6 -28 17.40 14.90 -8 6 28 12.60 14.80 8 6 -28 28.10 16.20 -7 -6 28 40.40 13.70 7 -6 -28 39.60 18.40 -7 -6 28 30.60 14.50 7 -6 -28 17.00 14.60 7 6 -28 62.39 18.50 -7 6 28 49.00 17.30 -6 -6 28 14.70 11.20 6 -6 -28 -1.00 15.10 -6 -6 28 11.50 12.40 6 -6 -28 16.20 14.10 6 6 -28 8.00 12.50 -6 6 28 2.40 12.90 5 -6 -28 177.08 23.00 5 -6 -28 167.18 25.50 -5 -6 28 177.38 23.50 -5 6 28 263.37 22.20 5 6 -28 153.78 22.80 -5 6 28 198.68 24.60 -4 -6 28 16.30 12.30 4 -6 -28 13.10 13.00 -4 -6 28 8.90 12.40 4 -6 -28 -0.60 13.40 -4 6 28 14.80 13.80 -4 6 28 -3.50 12.60 4 6 -28 14.80 15.00 -3 -6 28 7.90 12.80 -3 -6 28 4.20 12.00 3 -6 -28 21.00 15.00 3 -6 -28 10.10 12.90 -3 6 28 2.60 12.30 3 6 -28 28.70 14.60 -3 6 28 4.30 13.10 -2 -6 28 14.60 12.00 -2 -6 28 -0.50 11.70 2 -6 -28 -13.20 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6 -28 143.79 20.80 5 6 28 109.49 23.70 -6 -6 -28 13.00 14.30 -6 -6 -28 2.20 14.40 6 -6 28 22.20 16.80 -6 6 -28 34.80 18.50 6 6 28 -3.60 18.20 -6 6 -28 26.00 14.40 -11 -7 28 16.10 12.90 11 -7 -28 -19.70 16.80 -11 7 28 1.80 16.90 11 7 -28 -8.40 16.10 -11 7 28 -1.20 15.20 10 -7 -28 29.90 16.40 -10 -7 28 34.90 14.60 10 -7 -28 41.70 21.30 -10 7 28 14.00 16.60 10 7 -28 8.10 14.50 -9 -7 28 92.19 17.30 -9 -7 28 113.59 20.40 9 -7 -28 126.19 22.60 9 -7 -28 109.69 23.60 -9 7 28 120.09 23.70 9 7 -28 87.29 22.00 -8 -7 28 57.49 16.50 8 -7 -28 29.80 19.10 8 -7 -28 62.39 18.30 -8 -7 28 53.39 14.20 -8 7 28 52.99 19.00 8 7 -28 52.99 18.10 -7 -7 28 180.18 22.70 7 -7 -28 154.08 27.00 7 -7 -28 168.78 22.80 -7 -7 28 139.89 22.20 7 7 -28 177.38 25.00 -7 7 28 200.78 26.20 -6 -7 28 63.69 16.40 6 -7 -28 85.49 18.40 -6 -7 28 111.59 19.30 6 -7 -28 61.39 20.40 -6 7 28 133.19 21.70 6 7 -28 92.59 18.50 5 -7 -28 30.80 14.10 -5 -7 28 25.70 13.40 -5 -7 28 29.20 14.80 5 -7 -28 31.60 18.00 -5 7 28 29.30 14.90 -5 7 28 6.50 12.80 5 7 -28 25.50 15.30 -4 -7 28 28.50 14.30 4 -7 -28 37.20 14.80 4 -7 -28 40.10 17.70 -4 -7 28 36.30 13.80 4 7 -28 30.30 15.20 -4 7 28 38.00 14.90 -4 7 28 69.19 17.30 3 -7 -28 53.39 18.10 -3 -7 28 49.90 15.50 -3 -7 28 28.30 14.70 3 -7 -28 59.89 15.60 3 7 -28 47.00 17.20 -3 7 28 68.49 18.30 -3 7 28 54.19 16.10 -2 -7 28 222.08 25.20 -2 -7 28 201.88 24.80 2 -7 -28 184.08 22.50 2 -7 -28 131.09 22.00 2 7 -28 149.09 23.20 -2 7 28 219.68 23.60 -2 7 28 238.68 27.00 1 -7 -28 56.29 15.90 -1 -7 28 25.80 13.60 1 -7 -28 18.00 14.00 -1 -7 28 34.10 14.90 -1 7 28 26.60 13.50 1 7 -28 25.70 16.10 -1 7 28 11.00 16.30 0 -7 -28 -19.60 12.90 0 -7 28 5.90 12.80 0 -7 -28 4.40 12.60 0 -7 28 2.30 11.50 0 7 28 15.40 16.60 0 7 28 -1.70 10.90 0 7 -28 26.70 16.20 -1 -7 -28 22.50 13.80 1 -7 28 20.00 13.90 -1 -7 -28 31.80 15.00 -1 7 -28 9.40 15.80 1 7 28 29.20 16.40 -1 7 -28 28.70 15.30 1 7 28 38.20 12.90 -2 -7 -28 11.80 14.10 -2 -7 -28 -1.40 13.30 2 -7 28 14.30 12.80 2 7 28 -21.70 15.30 -2 7 -28 -0.70 14.70 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6 -8 -28 55.49 20.80 6 8 -28 91.19 20.20 -6 8 28 56.89 18.40 -5 -8 28 53.29 16.50 -5 -8 28 75.89 18.30 5 -8 -28 5.20 16.20 5 -8 -28 67.79 17.30 -5 8 28 47.30 17.70 5 8 -28 43.70 17.90 -5 8 28 26.90 15.10 4 -8 -28 55.49 15.30 -4 -8 28 14.80 12.40 4 -8 -28 21.00 16.50 -4 -8 28 37.40 14.50 -4 8 28 41.90 17.10 -4 8 28 90.69 19.30 4 8 -28 76.79 18.80 -3 -8 28 3.30 11.30 3 -8 -28 36.60 14.10 -3 -8 28 11.70 13.00 3 -8 -28 24.20 16.60 3 8 -28 12.80 14.30 -3 8 28 20.20 14.80 -3 8 28 29.40 15.60 2 -8 -28 7.90 14.80 -2 -8 28 -4.30 12.20 -2 -8 28 9.90 12.50 2 -8 -28 23.00 13.60 -2 8 28 -1.50 12.20 2 8 -28 -8.70 14.00 -2 8 28 15.10 15.50 -1 -8 28 16.60 13.50 1 -8 -28 8.70 14.70 1 -8 -28 26.00 14.40 -1 8 28 -9.70 15.20 1 8 -28 19.30 14.20 1 8 -28 -7.20 14.50 -1 8 28 24.60 14.30 0 -8 -28 87.79 20.00 0 -8 28 108.29 21.10 0 8 28 62.49 18.50 0 8 -28 115.79 22.30 0 8 -28 93.39 19.80 0 8 28 100.19 17.60 1 -8 28 -24.90 11.70 -1 -8 -28 -6.90 11.50 -1 8 -28 -13.90 13.50 1 8 28 23.70 12.80 1 8 28 6.70 16.60 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41.80 15.40 4 -9 -28 9.90 16.30 -4 -9 28 27.90 15.10 4 9 -28 3.80 14.10 -4 9 28 12.80 15.60 -4 9 28 17.70 16.10 3 -9 -28 10.90 16.60 -3 -9 28 9.80 13.70 -3 9 28 2.70 13.70 -3 9 28 37.20 17.10 3 9 -28 22.50 15.70 3 9 -28 15.80 15.40 2 -9 -28 62.09 20.80 -2 -9 28 60.79 17.10 -2 9 28 73.99 17.50 -2 9 28 77.99 20.70 2 9 -28 81.19 19.40 2 9 -28 75.69 18.80 -1 -9 28 9.10 13.10 1 -9 -28 -2.70 13.50 -1 9 28 10.40 14.00 1 9 -28 25.10 15.70 1 9 -28 26.20 17.30 -1 9 28 12.20 15.30 0 -9 -28 13.30 15.90 0 -9 28 38.40 15.60 0 9 28 20.40 18.00 0 9 -28 49.10 18.00 0 9 -28 33.40 17.20 0 9 28 29.70 14.80 1 -9 28 12.30 14.40 -1 -9 -28 5.00 14.80 1 9 28 15.70 18.60 -1 9 -28 13.30 15.60 -1 9 -28 27.10 15.90 -2 -9 -28 25.20 15.20 2 -9 28 26.20 15.20 2 9 28 6.60 19.20 -2 9 -28 39.00 16.80 -2 9 -28 39.10 17.70 -3 -9 -28 -7.00 13.90 3 -9 28 -3.10 13.30 3 9 28 27.00 20.70 -3 9 -28 -28.30 13.80 -3 9 -28 32.90 16.10 -4 -9 -28 -3.40 13.40 4 -9 28 11.10 14.00 -4 9 -28 -7.70 15.30 4 9 28 1.80 20.20 -4 9 -28 43.80 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-5 2 36 57.09 18.90 -5 2 36 47.40 16.70 5 2 -36 17.30 17.20 -4 -2 36 19.10 16.20 4 -2 -36 -8.20 15.50 -4 -2 36 18.50 16.90 4 -2 -36 28.50 17.60 4 2 -36 -9.50 14.10 -4 2 36 9.50 15.00 -4 2 36 1.80 14.60 3 -2 -36 26.20 17.40 -3 -2 36 1.80 14.80 3 -2 -36 -3.20 15.20 -3 -2 36 7.30 14.80 -3 2 36 -4.90 15.10 -3 2 36 2.90 14.10 3 2 -36 9.40 16.70 2 -2 -36 0.40 14.90 2 -2 -36 5.40 16.60 -2 -2 36 -22.10 13.10 -2 -2 36 6.00 14.40 2 2 -36 -21.70 15.30 -2 2 36 24.40 17.60 -2 2 36 23.50 16.80 -1 -2 36 17.40 16.10 1 -2 -36 26.90 18.30 -1 -2 36 38.00 17.30 1 2 -36 10.10 17.50 -1 2 36 35.00 17.30 -1 2 36 36.60 18.70 -5 -3 36 34.20 17.90 -5 -3 36 29.60 15.80 5 -3 -36 -2.50 16.00 -5 3 36 31.70 16.30 -5 3 36 29.30 17.60 4 -3 -36 -17.00 14.50 -4 -3 36 8.30 15.10 4 -3 -36 -11.40 14.10 -4 -3 36 8.90 13.60 4 3 -36 15.70 18.20 -4 3 36 35.10 17.00 -4 3 36 -11.40 13.60 3 -3 -36 -9.20 14.90 -3 -3 36 15.80 16.60 -3 -3 36 42.70 17.80 3 -3 -36 35.20 19.00 3 3 -36 12.20 17.50 -3 3 36 32.70 15.90 -3 3 36 46.30 17.90 -2 -3 36 -4.90 15.00 2 -3 -36 24.60 18.10 2 -3 -36 -11.50 14.30 -2 -3 36 31.30 16.60 -2 3 36 -9.40 15.90 2 3 -36 -9.50 14.70 -2 3 36 13.90 14.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 92233 _olex2_submission_special_instructions 'No special instructions were received'