data_Bi-macrodipa _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Justin J. Wilson' _publ_contact_author_address ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; _publ_contact_author_email jjw275@cornell.edu _publ_contact_author_phone 1(607)2554344 loop_ _publ_author_name _publ_author_address 'Hu, Aohan' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; 'Brown, Victoria' ;Department of Chemistry Simon Fraser University Burnaby, British Columbia V5A 1S6 Canada ; 'MacMillan, Samantha N.' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; 'Radchenko, Valery' ;Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada Department of Chemistry University of British Columbia Vancouver, British Columbia V6T 1Z1 Canada ; 'Yang, Hua' ;Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Wharton, Luke' ;Department of Chemistry University of British Columbia Vancouver, British Columbia V6T 1Z1 Canada Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Ramogida, Caterina F.' ;Department of Chemistry Simon Fraser University Burnaby, British Columbia V5A 1S6 Canada Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Wilson, Justin J.' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; _audit_creation_date 2020-01-16 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959) ; _shelx_SHELXL_version_number 2016/6 _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H34 Bi N4 O8, C2 F3 O2, H2 O' _chemical_formula_sum 'C28 H36 Bi F3 N4 O11' _chemical_formula_weight 870.59 _chemical_melting_point ? _chemical_oxdiff_formula C28H31BiF4N4O11 _chemical_oxdiff_usercomment 'Crystallized from Et2O/DMF.' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.08720(10) _cell_length_b 31.5764(3) _cell_length_c 10.82080(10) _cell_angle_alpha 90 _cell_angle_beta 94.0560(10) _cell_angle_gamma 90 _cell_volume 3097.16(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24667 _cell_measurement_temperature 99.97(18) _cell_measurement_theta_max 76.6360 _cell_measurement_theta_min 2.7820 _shelx_estimated_absorpt_T_max 0.694 _shelx_estimated_absorpt_T_min 0.223 _exptl_absorpt_coefficient_mu 11.930 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.205 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1720 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 20 1 0.0169 1 -20 0 0.0352 0 18 -3 0.0236 0 -17 4 0.0419 6 4 -1 0.0799 0 -2 -7 0.0483 0 2 7 0.0498 0 -20 -1 0.0187 -4 -15 0 0.0670 0 20 1 0.0075 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.033 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.3663 19.8599 0.7153 0.9578 -0.2299 -0.1728 1.1849 -20.0713 0.0550 -0.9706 0.2330 0.0611 -0.2366 17.9859 -3.3268 0.8807 -0.2118 0.4237 0.0588 -17.1439 3.8335 -0.8417 0.2024 -0.5006 5.7980 3.7527 -0.6131 0.2225 0.9262 0.3044 0.1428 -1.5918 -6.9962 -0.0649 -0.2712 0.9603 0.0328 1.7061 6.9801 0.0717 0.2994 -0.9514 -0.4294 -20.2287 -0.9768 -0.9872 -0.0776 0.1392 -4.0007 -14.9748 -0.2388 -0.7561 -0.6458 -0.1059 -0.1402 20.3733 0.7644 0.9908 -0.0259 -0.1325 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 44383 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.737 _diffrn_reflns_theta_min 2.799 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.97(18) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -39.00 21.00 0.50 0.05 -- -50.06 37.00 -90.00 120 2 \w -51.00 -13.00 0.50 0.20 -- -82.50 45.00-120.00 76 3 \w -82.00 -57.00 0.50 0.05 -- -50.06 138.00-150.00 50 4 \w -82.00 -57.00 0.50 0.20 -- -82.50 138.00-150.00 50 5 \w -77.00 -52.00 0.50 0.20 -- -82.50 131.00 33.00 50 6 \w -26.00 19.00 0.50 0.05 -- -50.06 19.00 150.00 90 7 \w 46.00 71.00 0.50 0.05 -- 50.06-131.00 -37.00 50 8 \w 53.00 78.00 0.50 0.20 -- 104.00-131.00 -37.00 50 9 \w 82.00 107.00 0.50 0.20 -- 104.00-106.00 -72.33 50 10 \w 79.00 106.00 0.50 0.20 -- 104.00 -94.00 -30.00 54 11 \w 79.00 104.00 0.50 0.20 -- 104.00 -94.00 0.00 50 12 \w 70.00 99.00 0.50 0.20 -- 104.00 -75.00 -55.73 58 13 \w 75.00 100.00 0.50 0.20 -- 104.00 -77.00 -90.00 50 14 \w 61.00 88.00 0.50 0.20 -- 104.00-125.00-120.00 54 15 \w 48.00 74.00 0.50 0.20 -- 104.00-102.00 -38.25 52 16 \w 53.00 106.00 0.50 0.20 -- 104.00 -98.00 -64.44 106 17 \w 51.00 100.00 0.50 0.20 -- 104.00 -94.00 30.00 98 18 \w 74.00 100.00 0.50 0.20 -- 104.00 -77.00 90.00 52 19 \w 88.00 121.00 0.50 0.20 -- 104.00-138.00 146.00 66 20 \w 100.00 125.00 0.50 0.20 -- 104.00-143.00 163.43 50 21 \w 55.00 94.00 0.50 0.20 -- 104.00-143.00 163.43 78 22 \w 54.00 102.00 0.50 0.05 -- 50.06-138.00 146.00 96 23 \w 48.00 74.00 0.50 0.20 -- 104.00 -94.00 150.00 52 24 \w 33.00 71.00 0.50 0.20 -- 104.00 -61.00 90.00 76 25 \w 33.00 59.00 0.50 0.20 -- 104.00 -61.00 30.00 52 26 \w 34.00 60.00 0.50 0.20 -- 104.00 -94.00 0.00 52 27 \w 32.00 67.00 0.50 0.20 -- 104.00 -75.00 -55.73 70 28 \w 45.00 76.00 0.50 0.20 -- 104.00-106.00 -72.33 62 29 \w 40.00 71.00 0.50 0.20 -- 104.00-104.00 -40.37 62 30 \w 43.00 68.00 0.50 0.20 -- 104.00 -61.00 -60.00 50 31 \w 32.00 100.00 0.50 0.20 -- 104.00 -77.00-120.00 136 32 \w 100.00 134.00 0.50 0.20 -- 104.00 15.00 0.00 68 33 \w 142.00 175.00 0.50 0.20 -- 104.00 15.00 0.00 66 34 \w 143.00 171.00 0.50 0.20 -- 104.00 101.00 130.77 56 35 \w 128.00 162.00 0.50 0.20 -- 104.00 125.00 150.00 68 36 \w 107.00 133.00 0.50 0.20 -- 104.00 101.00 130.77 52 37 \w 102.00 141.00 0.50 0.20 -- 104.00 131.00 33.00 78 38 \w 95.00 130.00 0.50 0.20 -- 104.00 61.00 30.00 70 39 \w 100.00 177.00 0.50 0.20 -- 104.00 30.00 52.31 154 40 \w 117.00 143.00 0.50 0.20 -- 104.00 125.00 -90.00 52 41 \w 107.00 133.00 0.50 0.20 -- 104.00 138.00-150.00 52 42 \w 104.00 176.00 0.50 0.20 -- 104.00 125.00-180.00 144 43 \w 138.00 164.00 0.50 0.20 -- 104.00 62.00-173.63 52 44 \w 111.00 169.00 0.50 0.20 -- 104.00 30.00-150.00 116 45 \w 118.00 145.00 0.50 0.20 -- 104.00 45.00-120.00 54 46 \w 92.00 124.00 0.50 0.20 -- 104.00 62.00-173.63 64 47 \w 84.00 140.00 0.50 0.20 -- 104.00 78.00-143.14 112 48 \w 32.00 57.00 0.50 0.20 -- 104.00 -61.00-150.00 50 49 \w -20.00 23.00 0.50 0.05 -- 50.06 -37.00-180.00 86 50 \w 65.00 111.00 0.50 0.20 -- 104.00-125.00 30.00 92 51 \w 104.00 176.00 0.50 0.20 -- 104.00 30.00 90.00 144 52 \w -118.00 -84.00 0.50 0.05 -- -50.06-138.00 146.00 68 53 \w -120.00 -95.00 0.50 0.05 -- -50.06-131.00 -37.00 50 54 \w -115.00 -75.00 0.50 0.05 -- -50.06-125.00 -60.00 80 55 \w -136.00-111.00 0.50 0.20 -- -82.50-131.00 -37.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0066460000 _diffrn_orient_matrix_UB_12 0.0487430000 _diffrn_orient_matrix_UB_13 -0.0016765000 _diffrn_orient_matrix_UB_21 0.1653657000 _diffrn_orient_matrix_UB_22 -0.0017302000 _diffrn_orient_matrix_UB_23 0.0425374000 _diffrn_orient_matrix_UB_31 0.0388178000 _diffrn_orient_matrix_UB_32 -0.0011264000 _diffrn_orient_matrix_UB_33 -0.1362149000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5426 _reflns_number_total 5604 _reflns_odcompleteness_completeness 98.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 77.83 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.873 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.112 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.366 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 491 _refine_ls_number_reflns 5604 _refine_ls_number_restraints 351 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0374 _refine_ls_restrained_S_all 1.332 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+17.6906P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.0946 _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 O(H,H) groups 2. Restrained distances C1B-F2 \\sim C1B-F3 \\sim C1B-F1 with sigma of 0.02 C27-F2 \\sim C27-F3 \\sim C27-F1 with sigma of 0.04 F2-F3 \\sim F3-F1 \\sim F1-F2 with sigma of 0.04 C27-O10 \\sim C27-O9 with sigma of 0.02 C27A-F2A \\sim C27A-F3A \\sim C27A-F1A with sigma of 0.04 C1D-F2A \\sim C1D-F3A \\sim C1D-F1A with sigma of 0.02 F2A-F3A \\sim F3A-F1A \\sim F1A-F2A with sigma of 0.04 C27A-O10A \\sim C27A-O9A with sigma of 0.02 3. Restrained planarity O9, O10, C1B, C27 with sigma of 0.1 O9A, O10A, C1D, C27A with sigma of 0.1 4. Uiso/Uaniso restraints and constraints F1 \\sim F2 \\sim F3 \\sim O9 \\sim O10 \\sim C1B \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A F1A \\sim F2A \\sim F3A \\sim O9A \\sim O10A \\sim C1D \\sim C27A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A F1 \\sim F2 \\sim F3 \\sim O9 \\sim O10 \\sim C1B \\sim C27 \\sim F1A \\sim F2A \\sim F3A \\sim O9A \\sim O10A \\sim C1D \\sim C27A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 5. Rigid body (RIGU) restrains F1, F2, F3, O9, O10, C1B, C27 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 F1A, F2A, F3A, O9A, O10A, C1D, C27A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 F1, F2, F3, O9, O10, C1B, C27, F1A, F2A, F3A, O9A, O10A, C1D, C27A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Same fragment restrains {F1A, F2A, F3A, O9A, O10A, C1D, C27A} sigma for 1-2: 0.02, 1-3: 0.04 as in {F1, F2, F3, O9, O10, C1B, C27} 7. Others Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O9A)=Sof(O10A)=Sof(C1D)=Sof(C27A)=1-FVAR(1) Sof(F1)=Sof(F2)=Sof(F3)=Sof(O9)=Sof(O10)=Sof(C1B)=Sof(C27)=FVAR(1) 8.a Free rotating group: O11(H11C,H11D) 8.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C20(H20A,H20B) 8.c Aromatic/amide H refined with riding coordinates: C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24) ; _atom_sites_solution_hydrogens mixed _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 Bi Bi 0.33348(2) 0.61800(2) 0.29316(2) 0.02824(10) Uani 1 1 d . . . . . O1 O 0.1516(5) 0.68209(19) 0.3307(5) 0.0465(13) Uani 1 1 d . . . . . O2 O 0.4975(5) 0.63860(14) 0.0482(4) 0.0299(9) Uani 1 1 d . . . . . O3 O 0.4552(5) 0.55334(14) 0.0677(4) 0.0272(9) Uani 1 1 d . . . . . O4 O 0.1570(5) 0.57073(16) 0.0889(4) 0.0318(10) Uani 1 1 d . . . . . O5 O 0.5588(4) 0.58636(13) 0.3245(4) 0.0256(9) Uani 1 1 d . . . . . O6 O 0.6895(5) 0.52709(15) 0.3167(4) 0.0360(10) Uani 1 1 d . . . . . O7 O 0.3124(5) 0.61050(17) 0.4938(4) 0.0367(11) Uani 1 1 d . . . . . O8 O 0.4028(5) 0.61475(16) 0.6882(4) 0.0366(11) Uani 1 1 d . . . . . N1 N 0.0587(6) 0.5964(2) 0.3254(5) 0.0453(16) Uani 1 1 d . . . . . N2 N 0.4065(7) 0.70324(19) 0.2007(5) 0.0376(14) Uani 1 1 d . . . . . N3 N 0.3097(6) 0.54386(19) 0.3345(4) 0.0325(13) Uani 1 1 d . . . . . N4 N 0.4999(5) 0.66713(16) 0.4190(4) 0.0244(10) Uani 1 1 d . . . . . C1 C -0.0021(8) 0.6284(4) 0.4095(8) 0.061(3) Uani 1 1 d . . . . . H1A H -0.106452 0.621290 0.420714 0.073 Uiso 1 1 calc R U . . . H1B H 0.052807 0.626438 0.491648 0.073 Uiso 1 1 calc R U . . . C2 C 0.0052(8) 0.6720(4) 0.3656(8) 0.068(3) Uani 1 1 d . . . . . H2A H -0.066562 0.675914 0.293320 0.081 Uiso 1 1 calc R U . . . H2B H -0.022013 0.691531 0.431820 0.081 Uiso 1 1 calc R U . . . C3 C 0.1560(10) 0.7212(3) 0.2634(8) 0.059(3) Uani 1 1 d . . . . . H3A H 0.099643 0.743257 0.304827 0.071 Uiso 1 1 calc R U . . . H3B H 0.110705 0.717328 0.178222 0.071 Uiso 1 1 calc R U . . . C4 C 0.3126(10) 0.7346(3) 0.2590(7) 0.050(2) Uani 1 1 d . . . . . H4A H 0.315735 0.761566 0.212634 0.060 Uiso 1 1 calc R U . . . H4B H 0.354208 0.740006 0.344622 0.060 Uiso 1 1 calc R U . . . C5 C 0.3777(11) 0.7053(3) 0.0650(6) 0.049(2) Uani 1 1 d . . . . . H5A H 0.383015 0.735294 0.038579 0.059 Uiso 1 1 calc R U . . . H5B H 0.276054 0.695224 0.043005 0.059 Uiso 1 1 calc R U . . . C6 C 0.4833(10) 0.6797(2) -0.0057(6) 0.0412(17) Uani 1 1 d . . . . . H6A H 0.445896 0.677323 -0.093592 0.049 Uiso 1 1 calc R U . . . H6B H 0.580791 0.693790 -0.002386 0.049 Uiso 1 1 calc R U . . . C7 C 0.5854(7) 0.6124(2) -0.0245(6) 0.0293(13) Uani 1 1 d . . . . . H7A H 0.685671 0.624471 -0.026633 0.035 Uiso 1 1 calc R U . . . H7B H 0.540740 0.610700 -0.110470 0.035 Uiso 1 1 calc R U . . . C8 C 0.5938(7) 0.5688(2) 0.0326(5) 0.0274(13) Uani 1 1 d . . . . . H8A H 0.633078 0.548805 -0.027364 0.033 Uiso 1 1 calc R U . . . H8B H 0.664046 0.569479 0.106826 0.033 Uiso 1 1 calc R U . . . C9 C 0.3503(7) 0.5490(2) -0.0347(5) 0.0275(13) Uani 1 1 d . . . . . H9A H 0.381907 0.526563 -0.091043 0.033 Uiso 1 1 calc R U . . . H9B H 0.341466 0.575903 -0.081532 0.033 Uiso 1 1 calc R U . . . C10 C 0.2045(7) 0.5375(2) 0.0132(6) 0.0307(14) Uani 1 1 d . . . . . H10A H 0.130550 0.532798 -0.057106 0.037 Uiso 1 1 calc R U . . . H10B H 0.214384 0.511015 0.061921 0.037 Uiso 1 1 calc R U . . . C11 C 0.0082(8) 0.5647(3) 0.1158(7) 0.0433(18) Uani 1 1 d . . . . . H11A H -0.004348 0.536421 0.153021 0.052 Uiso 1 1 calc R U . . . H11B H -0.057175 0.566579 0.038821 0.052 Uiso 1 1 calc R U . . . C12 C -0.0306(8) 0.5988(3) 0.2053(6) 0.0451(19) Uani 1 1 d . . . . . H12A H -0.015479 0.626849 0.167273 0.054 Uiso 1 1 calc R U . . . H12B H -0.136407 0.596335 0.220664 0.054 Uiso 1 1 calc R U . . . C13 C 0.0553(8) 0.5537(3) 0.3817(7) 0.050(2) Uani 1 1 d . . . . . H13A H -0.039699 0.540061 0.354797 0.061 Uiso 1 1 calc R U . . . H13B H 0.058622 0.556876 0.472883 0.061 Uiso 1 1 calc R U . . . C14 C 0.1792(8) 0.5248(3) 0.3498(6) 0.0430(19) Uani 1 1 d . . . . . C15 C 0.1690(10) 0.4810(3) 0.3490(7) 0.054(2) Uani 1 1 d . . . . . H15 H 0.075952 0.467741 0.354717 0.064 Uiso 1 1 calc R U . . . C16 C 0.2932(9) 0.4568(3) 0.3401(7) 0.048(2) Uani 1 1 d . . . . . H16 H 0.286542 0.426797 0.339840 0.057 Uiso 1 1 calc R U . . . C17 C 0.4286(9) 0.4765(2) 0.3315(6) 0.0399(17) Uani 1 1 d . . . . . H17 H 0.516684 0.460514 0.327910 0.048 Uiso 1 1 calc R U . . . C18 C 0.4307(7) 0.5204(2) 0.3284(5) 0.0290(13) Uani 1 1 d . . . . . C19 C 0.5720(7) 0.5456(2) 0.3219(5) 0.0276(13) Uani 1 1 d . . . . . C20 C 0.5614(9) 0.7091(2) 0.2425(6) 0.0374(16) Uani 1 1 d . . . . . H20A H 0.589797 0.739030 0.230560 0.045 Uiso 1 1 calc R U . . . H20B H 0.623843 0.691134 0.192568 0.045 Uiso 1 1 calc R U . . . C21 C 0.5867(7) 0.69750(19) 0.3776(5) 0.0251(12) Uani 1 1 d . . . . . C22 C 0.6958(7) 0.7169(2) 0.4552(6) 0.0303(14) Uani 1 1 d . . . . . H22 H 0.755658 0.738687 0.424736 0.036 Uiso 1 1 calc R U . . . C23 C 0.7152(7) 0.7041(2) 0.5765(6) 0.0308(14) Uani 1 1 d . . . . . H23 H 0.791493 0.716165 0.629697 0.037 Uiso 1 1 calc R U . . . C24 C 0.6243(7) 0.6737(2) 0.6210(6) 0.0279(13) Uani 1 1 d . . . . . H24 H 0.634907 0.664835 0.705088 0.033 Uiso 1 1 calc R U . . . C25 C 0.5165(6) 0.65636(19) 0.5389(5) 0.0240(12) Uani 1 1 d . . . . . C26 C 0.4050(7) 0.6249(2) 0.5792(5) 0.0302(14) Uani 1 1 d . . . . . F1 F 1.138(2) 0.6362(8) 0.884(2) 0.077(5) Uani 0.62(4) 1 d D U P A 1 F2 F 0.931(2) 0.6188(6) 0.796(2) 0.091(6) Uani 0.62(4) 1 d D U P A 1 F3 F 1.056(2) 0.6695(7) 0.7211(14) 0.077(5) Uani 0.62(4) 1 d D U P A 1 O9 O 0.871(3) 0.7106(6) 0.8446(12) 0.059(5) Uani 0.62(4) 1 d D U P A 1 O10 O 0.936(3) 0.6777(5) 1.0181(9) 0.063(5) Uani 0.62(4) 1 d D U P A 1 C1B C 1.0165(16) 0.6522(5) 0.8268(13) 0.048(3) Uani 0.62(4) 1 d D U P A 1 C27 C 0.9327(13) 0.6834(4) 0.9066(10) 0.026(3) Uani 0.62(4) 1 d D U P A 1 F1A F 1.159(3) 0.6466(13) 0.864(4) 0.084(8) Uani 0.38(4) 1 d D U P A 2 F2A F 0.952(4) 0.6118(8) 0.840(3) 0.081(6) Uani 0.38(4) 1 d D U P A 2 F3A F 1.006(4) 0.6567(12) 0.7074(18) 0.090(9) Uani 0.38(4) 1 d D U P A 2 O9A O 0.819(2) 0.6932(10) 0.857(2) 0.048(7) Uani 0.38(4) 1 d D U P A 2 O10A O 1.004(3) 0.6962(14) 1.000(3) 0.083(10) Uani 0.38(4) 1 d D U P A 2 C1D C 1.016(3) 0.6497(8) 0.8294(19) 0.055(5) Uani 0.38(4) 1 d D U P A 2 C27A C 0.939(2) 0.6839(7) 0.9043(17) 0.038(6) Uani 0.38(4) 1 d D U P A 2 O11 O 0.1645(5) 0.54946(17) 0.6903(5) 0.0420(12) Uani 1 1 d G . . . . H11C H 0.221298 0.527271 0.692349 0.063 Uiso 1 1 d G U . . . H11D H 0.225101 0.570801 0.697381 0.063 Uiso 1 1 d G 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 Bi 0.02299(13) 0.04578(16) 0.01627(13) -0.00074(10) 0.00363(8) -0.00052(11) O1 0.032(3) 0.071(4) 0.036(3) -0.013(3) 0.001(2) 0.017(3) O2 0.039(2) 0.032(2) 0.020(2) 0.0013(17) 0.0065(17) 0.0013(19) O3 0.025(2) 0.038(2) 0.0183(19) 0.0042(17) 0.0016(16) -0.0005(18) O4 0.021(2) 0.052(3) 0.023(2) -0.0107(19) 0.0037(17) -0.0071(19) O5 0.021(2) 0.031(2) 0.024(2) 0.0013(17) -0.0016(16) -0.0041(17) O6 0.026(2) 0.033(2) 0.048(3) 0.007(2) -0.004(2) -0.001(2) O7 0.035(2) 0.061(3) 0.015(2) -0.003(2) 0.0047(17) -0.017(2) O8 0.042(3) 0.047(3) 0.020(2) 0.0036(19) 0.0014(18) -0.008(2) N1 0.025(3) 0.085(5) 0.026(3) -0.013(3) 0.009(2) -0.006(3) N2 0.061(4) 0.036(3) 0.016(2) 0.003(2) 0.006(2) 0.019(3) N3 0.031(3) 0.050(3) 0.017(2) 0.002(2) 0.004(2) -0.019(3) N4 0.023(3) 0.029(3) 0.021(2) -0.003(2) 0.0032(19) 0.000(2) C1 0.012(3) 0.130(10) 0.042(4) -0.043(5) 0.006(3) -0.004(4) C2 0.017(3) 0.138(10) 0.048(5) -0.047(6) -0.004(3) 0.018(5) C3 0.059(6) 0.078(6) 0.038(4) -0.015(4) -0.008(4) 0.042(5) C4 0.073(6) 0.047(5) 0.028(4) -0.001(3) -0.005(3) 0.034(4) C5 0.086(6) 0.042(4) 0.020(3) 0.006(3) 0.004(3) 0.020(4) C6 0.070(5) 0.036(4) 0.018(3) 0.004(3) 0.008(3) 0.007(4) C7 0.031(3) 0.035(4) 0.022(3) -0.001(2) 0.007(2) -0.003(3) C8 0.025(3) 0.036(3) 0.022(3) -0.002(2) 0.004(2) -0.001(3) C9 0.029(3) 0.032(3) 0.022(3) -0.002(2) 0.002(2) -0.002(3) C10 0.032(3) 0.037(4) 0.023(3) -0.006(3) 0.002(2) -0.008(3) C11 0.027(3) 0.074(5) 0.030(3) -0.014(3) 0.005(3) -0.009(3) C12 0.027(4) 0.080(6) 0.029(3) -0.014(4) 0.004(3) -0.001(4) C13 0.024(4) 0.099(7) 0.028(3) 0.001(4) 0.004(3) -0.029(4) C14 0.034(4) 0.078(6) 0.017(3) 0.004(3) 0.003(3) -0.023(4) C15 0.053(5) 0.079(6) 0.029(4) 0.015(4) 0.003(3) -0.040(5) C16 0.045(5) 0.058(5) 0.041(4) 0.013(4) 0.003(3) -0.025(4) C17 0.044(4) 0.044(4) 0.031(3) 0.010(3) -0.003(3) -0.013(3) C18 0.028(3) 0.039(4) 0.020(3) 0.006(3) 0.000(2) -0.007(3) C19 0.029(3) 0.036(4) 0.017(3) 0.009(2) -0.004(2) -0.007(3) C20 0.052(4) 0.031(4) 0.030(3) -0.001(3) 0.014(3) -0.006(3) C21 0.026(3) 0.026(3) 0.024(3) 0.000(2) 0.005(2) 0.005(2) C22 0.029(3) 0.025(3) 0.038(4) 0.000(3) 0.014(3) 0.006(3) C23 0.022(3) 0.032(3) 0.038(3) -0.006(3) 0.002(3) 0.004(3) C24 0.026(3) 0.033(3) 0.025(3) 0.001(2) 0.002(2) 0.006(3) C25 0.023(3) 0.028(3) 0.021(3) -0.002(2) 0.000(2) 0.002(2) C26 0.031(3) 0.039(4) 0.021(3) -0.003(3) 0.006(2) -0.007(3) F1 0.067(7) 0.098(10) 0.064(9) -0.005(7) -0.015(6) 0.055(7) F2 0.094(8) 0.062(8) 0.113(14) -0.054(8) -0.019(8) 0.009(7) F3 0.075(9) 0.117(10) 0.039(6) -0.013(5) 0.012(5) 0.026(7) O9 0.087(11) 0.044(8) 0.047(5) 0.004(5) 0.003(6) 0.036(7) O10 0.084(11) 0.077(9) 0.028(4) -0.002(4) 0.004(5) 0.020(8) C1B 0.048(7) 0.054(7) 0.039(6) -0.013(5) -0.010(5) 0.020(5) C27 0.020(6) 0.026(6) 0.032(5) 0.001(4) -0.002(5) -0.002(5) F1A 0.061(9) 0.13(2) 0.057(13) -0.011(14) -0.006(8) 0.057(9) F2A 0.105(13) 0.056(8) 0.075(15) -0.028(8) -0.030(10) 0.035(8) F3A 0.108(19) 0.133(19) 0.027(7) -0.012(9) -0.004(8) 0.087(15) O9A 0.047(9) 0.054(14) 0.041(10) -0.021(9) -0.011(7) 0.019(8) O10A 0.068(14) 0.13(2) 0.052(11) -0.050(13) -0.015(10) 0.026(14) C1D 0.065(9) 0.066(9) 0.030(8) -0.010(8) -0.014(8) 0.039(8) C27A 0.041(10) 0.043(11) 0.029(8) -0.004(8) -0.001(7) 0.011(9) O11 0.033(3) 0.044(3) 0.049(3) 0.000(2) 0.003(2) -0.003(2) _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 Bi O1 2.663(5) . ? Bi O5 2.282(4) . ? Bi O7 2.206(4) . ? Bi N1 2.635(6) . ? Bi N3 2.396(6) . ? Bi N4 2.501(5) . ? O1 C2 1.444(10) . ? O1 C3 1.436(11) . ? O2 C6 1.425(8) . ? O2 C7 1.425(7) . ? O3 C8 1.426(7) . ? O3 C9 1.417(7) . ? O4 C10 1.416(8) . ? O4 C11 1.416(8) . ? O5 C19 1.292(8) . ? O6 C19 1.223(8) . ? O7 C26 1.288(8) . ? O8 C26 1.224(8) . ? N1 C1 1.493(10) . ? N1 C12 1.485(9) . ? N1 C13 1.480(12) . ? N2 C4 1.477(9) . ? N2 C5 1.475(8) . ? N2 C20 1.460(10) . ? N3 C14 1.350(9) . ? N3 C18 1.332(9) . ? N4 C21 1.340(8) . ? N4 C25 1.339(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.459(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.489(14) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.506(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.509(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.501(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.507(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.509(13) . ? C14 C15 1.386(13) . ? C15 H15 0.9500 . ? C15 C16 1.372(14) . ? C16 H16 0.9500 . ? C16 C17 1.388(10) . ? C17 H17 0.9500 . ? C17 C18 1.385(10) . ? C18 C19 1.517(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.508(9) . ? C21 C22 1.395(10) . ? C22 H22 0.9500 . ? C22 C23 1.373(10) . ? C23 H23 0.9500 . ? C23 C24 1.376(9) . ? C24 H24 0.9500 . ? C24 C25 1.387(9) . ? C25 C26 1.505(9) . ? F1 C1B 1.326(12) . ? F2 C1B 1.339(12) . ? F3 C1B 1.340(12) . ? O9 C27 1.203(11) . ? O10 C27 1.218(11) . ? C1B C27 1.545(12) . ? F1A C1D 1.331(14) . ? F2A C1D 1.337(14) . ? F3A C1D 1.336(14) . ? O9A C27A 1.211(14) . ? O10A C27A 1.222(14) . ? C1D C27A 1.549(15) . ? O11 H11C 0.8696 . ? O11 H11D 0.8703 . ? 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 O5 Bi O1 150.49(16) . . ? O5 Bi N1 135.7(2) . . ? O5 Bi N3 68.67(17) . . ? O5 Bi N4 71.88(16) . . ? O7 Bi O1 80.40(18) . . ? O7 Bi O5 86.90(17) . . ? O7 Bi N1 72.12(18) . . ? O7 Bi N3 72.31(18) . . ? O7 Bi N4 67.78(16) . . ? N1 Bi O1 64.7(2) . . ? N3 Bi O1 130.47(18) . . ? N3 Bi N1 67.9(2) . . ? N3 Bi N4 124.28(17) . . ? N4 Bi O1 78.66(16) . . ? N4 Bi N1 129.09(17) . . ? C2 O1 Bi 117.7(6) . . ? C3 O1 Bi 122.4(4) . . ? C3 O1 C2 112.5(7) . . ? C6 O2 C7 109.9(5) . . ? C9 O3 C8 112.5(4) . . ? C10 O4 C11 110.7(5) . . ? C19 O5 Bi 121.1(4) . . ? C26 O7 Bi 124.8(4) . . ? C1 N1 Bi 107.5(5) . . ? C12 N1 Bi 109.6(4) . . ? C12 N1 C1 107.2(6) . . ? C13 N1 Bi 109.7(4) . . ? C13 N1 C1 110.2(7) . . ? C13 N1 C12 112.4(6) . . ? C5 N2 C4 109.2(6) . . ? C20 N2 C4 110.8(6) . . ? C20 N2 C5 113.7(6) . . ? C14 N3 Bi 123.4(6) . . ? C18 N3 Bi 116.7(4) . . ? C18 N3 C14 119.5(7) . . ? C21 N4 Bi 127.6(4) . . ? C25 N4 Bi 113.1(4) . . ? C25 N4 C21 118.5(5) . . ? N1 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C2 C1 N1 114.4(7) . . ? C2 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? O1 C2 C1 110.9(7) . . ? O1 C2 H2A 109.4 . . ? O1 C2 H2B 109.4 . . ? C1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O1 C3 H3A 109.9 . . ? O1 C3 H3B 109.9 . . ? O1 C3 C4 108.7(6) . . ? H3A C3 H3B 108.3 . . ? C4 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? N2 C4 C3 113.9(7) . . ? N2 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C3 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N2 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N2 C5 C6 114.0(6) . . ? H5A C5 H5B 107.6 . . ? C6 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? O2 C6 C5 108.9(6) . . ? O2 C6 H6A 109.9 . . ? O2 C6 H6B 109.9 . . ? C5 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O2 C7 H7A 110.0 . . ? O2 C7 H7B 110.0 . . ? O2 C7 C8 108.5(5) . . ? H7A C7 H7B 108.4 . . ? C8 C7 H7A 110.0 . . ? C8 C7 H7B 110.0 . . ? O3 C8 C7 113.6(5) . . ? O3 C8 H8A 108.8 . . ? O3 C8 H8B 108.8 . . ? C7 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O3 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? O3 C9 C10 108.4(5) . . ? H9A C9 H9B 108.4 . . ? C10 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? O4 C10 C9 109.5(5) . . ? O4 C10 H10A 109.8 . . ? O4 C10 H10B 109.8 . . ? C9 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? O4 C11 H11A 110.1 . . ? O4 C11 H11B 110.1 . . ? O4 C11 C12 107.9(6) . . ? H11A C11 H11B 108.4 . . ? C12 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? N1 C12 C11 112.8(7) . . ? N1 C12 H12A 109.0 . . ? N1 C12 H12B 109.0 . . ? C11 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N1 C13 H13A 108.6 . . ? N1 C13 H13B 108.6 . . ? N1 C13 C14 114.7(5) . . ? H13A C13 H13B 107.6 . . ? C14 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? N3 C14 C13 115.8(7) . . ? N3 C14 C15 120.2(8) . . ? C15 C14 C13 123.7(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 120.1(7) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 120.2 . . ? C15 C16 C17 119.5(8) . . ? C17 C16 H16 120.2 . . ? C16 C17 H17 121.2 . . ? C18 C17 C16 117.6(8) . . ? C18 C17 H17 121.2 . . ? N3 C18 C17 122.8(6) . . ? N3 C18 C19 114.4(6) . . ? C17 C18 C19 122.7(6) . . ? O5 C19 C18 116.2(6) . . ? O6 C19 O5 124.1(6) . . ? O6 C19 C18 119.6(6) . . ? N2 C20 H20A 109.6 . . ? N2 C20 H20B 109.6 . . ? N2 C20 C21 110.3(5) . . ? H20A C20 H20B 108.1 . . ? C21 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? N4 C21 C20 116.5(6) . . ? N4 C21 C22 121.5(5) . . ? C22 C21 C20 122.0(6) . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.9(6) . . ? C23 C22 H22 120.6 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.1(6) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 121.2 . . ? C23 C24 C25 117.7(6) . . ? C25 C24 H24 121.2 . . ? N4 C25 C24 123.1(6) . . ? N4 C25 C26 114.6(5) . . ? C24 C25 C26 122.3(5) . . ? O7 C26 C25 116.4(5) . . ? O8 C26 O7 122.9(6) . . ? O8 C26 C25 120.6(6) . . ? F1 C1B F2 105.3(12) . . ? F1 C1B F3 107.1(13) . . ? F1 C1B C27 113.9(12) . . ? F2 C1B F3 107.1(12) . . ? F2 C1B C27 110.0(11) . . ? F3 C1B C27 112.9(11) . . ? O9 C27 O10 129.5(12) . . ? O9 C27 C1B 111.8(10) . . ? O10 C27 C1B 118.7(10) . . ? F1A C1D F2A 109.3(18) . . ? F1A C1D F3A 106.6(17) . . ? F1A C1D C27A 111.9(17) . . ? F2A C1D C27A 111.4(16) . . ? F3A C1D F2A 103.6(17) . . ? F3A C1D C27A 113.5(15) . . ? O9A C27A O10A 130.6(19) . . ? O9A C27A C1D 112.2(15) . . ? O10A C27A C1D 117.2(16) . . ? H11C O11 H11D 104.5 . . ? 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 O11 H11C O6 0.87 1.90 2.761(7) 168.3 3_666 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 Bi O1 C2 C1 17.0(8) . . . . ? Bi O1 C3 C4 -44.8(8) . . . . ? Bi O5 C19 O6 166.9(5) . . . . ? Bi O5 C19 C18 -14.3(6) . . . . ? Bi O7 C26 O8 -168.3(5) . . . . ? Bi O7 C26 C25 13.2(8) . . . . ? Bi N1 C1 C2 56.7(7) . . . . ? Bi N1 C12 C11 70.0(7) . . . . ? Bi N1 C13 C14 -29.4(7) . . . . ? Bi N3 C14 C13 -19.6(7) . . . . ? Bi N3 C14 C15 167.3(5) . . . . ? Bi N3 C18 C17 -170.0(5) . . . . ? Bi N3 C18 C19 11.9(6) . . . . ? Bi N4 C21 C20 12.4(8) . . . . ? Bi N4 C21 C22 -166.9(4) . . . . ? Bi N4 C25 C24 167.1(5) . . . . ? Bi N4 C25 C26 -15.0(6) . . . . ? O1 C3 C4 N2 58.5(8) . . . . ? O2 C7 C8 O3 44.9(7) . . . . ? O3 C9 C10 O4 62.5(7) . . . . ? O4 C11 C12 N1 -62.7(9) . . . . ? N1 C1 C2 O1 -50.1(9) . . . . ? N1 C13 C14 N3 33.5(8) . . . . ? N1 C13 C14 C15 -153.6(7) . . . . ? N2 C5 C6 O2 47.3(10) . . . . ? N2 C20 C21 N4 31.0(8) . . . . ? N2 C20 C21 C22 -149.7(6) . . . . ? N3 C14 C15 C16 3.8(10) . . . . ? N3 C18 C19 O5 0.8(7) . . . . ? N3 C18 C19 O6 179.6(5) . . . . ? N4 C21 C22 C23 0.8(9) . . . . ? N4 C25 C26 O7 3.4(8) . . . . ? N4 C25 C26 O8 -175.2(6) . . . . ? C1 N1 C12 C11 -173.6(7) . . . . ? C1 N1 C13 C14 -147.6(6) . . . . ? C2 O1 C3 C4 165.9(6) . . . . ? C3 O1 C2 C1 167.8(6) . . . . ? C4 N2 C5 C6 171.0(7) . . . . ? C4 N2 C20 C21 68.5(7) . . . . ? C5 N2 C4 C3 77.2(8) . . . . ? C5 N2 C20 C21 -168.1(6) . . . . ? C6 O2 C7 C8 -178.1(6) . . . . ? C7 O2 C6 C5 174.2(6) . . . . ? C8 O3 C9 C10 -173.5(5) . . . . ? C9 O3 C8 C7 62.0(7) . . . . ? C10 O4 C11 C12 175.0(6) . . . . ? C11 O4 C10 C9 168.7(6) . . . . ? C12 N1 C1 C2 -61.1(8) . . . . ? C12 N1 C13 C14 92.9(7) . . . . ? C13 N1 C1 C2 176.3(6) . . . . ? C13 N1 C12 C11 -52.4(8) . . . . ? C13 C14 C15 C16 -168.7(7) . . . . ? C14 N3 C18 C17 2.9(9) . . . . ? C14 N3 C18 C19 -175.2(5) . . . . ? C14 C15 C16 C17 -0.2(11) . . . . ? C15 C16 C17 C18 -2.0(10) . . . . ? C16 C17 C18 N3 0.7(10) . . . . ? C16 C17 C18 C19 178.6(6) . . . . ? C17 C18 C19 O5 -177.3(6) . . . . ? C17 C18 C19 O6 1.5(9) . . . . ? C18 N3 C14 C13 168.0(6) . . . . ? C18 N3 C14 C15 -5.2(9) . . . . ? C20 N2 C4 C3 -156.8(6) . . . . ? C20 N2 C5 C6 46.7(9) . . . . ? C20 C21 C22 C23 -178.4(6) . . . . ? C21 N4 C25 C24 -3.3(9) . . . . ? C21 N4 C25 C26 174.6(5) . . . . ? C21 C22 C23 C24 -2.5(9) . . . . ? C22 C23 C24 C25 1.3(9) . . . . ? C23 C24 C25 N4 1.7(9) . . . . ? C23 C24 C25 C26 -176.1(6) . . . . ? C24 C25 C26 O7 -178.7(6) . . . . ? C24 C25 C26 O8 2.8(10) . . . . ? C25 N4 C21 C20 -178.7(5) . . . . ? C25 N4 C21 C22 2.0(8) . . . . ? F1 C1B C27 O9 148.3(16) . . . . ? F1 C1B C27 O10 -32.0(18) . . . . ? F2 C1B C27 O9 -93.7(16) . . . . ? F2 C1B C27 O10 85.9(16) . . . . ? F3 C1B C27 O9 25.9(17) . . . . ? F3 C1B C27 O10 -154.4(15) . . . . ? F1A C1D C27A O9A 166(2) . . . . ? F1A C1D C27A O10A -17(3) . . . . ? F2A C1D C27A O9A -72(2) . . . . ? F2A C1D C27A O10A 106(3) . . . . ? F3A C1D C27A O9A 45(3) . . . . ? F3A C1D C27A O10A -137(3) . . . . ? _shelx_res_file ; TITL rah14_abs_a.res in P2(1)/c rah14_abs.res created by SHELXL-2016/6 at 14:15:40 on 16-Jan-2020 REM Old TITL Rah14_abs in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.139, Rweak 0.075, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C31 N2 O10 F3 Bi CELL 1.54184 9.0872 31.5764 10.8208 90 94.056 90 ZERR 4 0.0001 0.0003 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Bi F N O UNIT 112 144 4 12 16 44 EQIV $1 1-X,1-Y,1-Z SADI C1B F2 C1B F3 C1B F1 FLAT O9 O10 C1B C27 SADI 0.04 C27 F2 C27 F3 C27 F1 RIGU F1 > C27 SADI 0.04 F2 F3 F3 F1 F1 F2 SIMU F1 > C27 SADI C27 O10 C27 O9 SADI 0.04 C27A F2A C27A F3A C27A F1A SADI C1D F2A C1D F3A C1D F1A FLAT O9A O10A C1D C27A SADI 0.04 F2A F3A F3A F1A F1A F2A SIMU F1A > C27A RIGU F1A > C27A SADI C27A O10A C27A O9A SIMU F1 > C27A RIGU F1 > C27A L.S. 10 PLAN 40 SIZE 0.033 0.103 0.18 TEMP -173 CONF HTAB O11 O6_$1 BOND $H list 4 fmap 2 53 MORE -1 ACTA SHEL 100 0.833 REM REM REM WGHT 0.000000 17.690601 FVAR 0.24289 0.62168 BI 3 0.333475 0.617997 0.293162 11.00000 0.02299 0.04578 = 0.01627 -0.00074 0.00363 -0.00052 O1 6 0.151564 0.682093 0.330732 11.00000 0.03180 0.07122 = 0.03616 -0.01290 0.00100 0.01678 O2 6 0.497501 0.638595 0.048247 11.00000 0.03916 0.03174 = 0.01954 0.00125 0.00646 0.00126 O3 6 0.455210 0.553341 0.067708 11.00000 0.02498 0.03844 = 0.01830 0.00418 0.00155 -0.00053 O4 6 0.157048 0.570730 0.088855 11.00000 0.02067 0.05181 = 0.02333 -0.01073 0.00365 -0.00714 O5 6 0.558778 0.586364 0.324542 11.00000 0.02141 0.03094 = 0.02394 0.00130 -0.00158 -0.00411 O6 6 0.689500 0.527088 0.316734 11.00000 0.02557 0.03313 = 0.04834 0.00698 -0.00357 -0.00089 O7 6 0.312410 0.610501 0.493828 11.00000 0.03475 0.06126 = 0.01453 -0.00274 0.00466 -0.01692 O8 6 0.402776 0.614748 0.688177 11.00000 0.04202 0.04731 = 0.02030 0.00357 0.00142 -0.00831 N1 5 0.058706 0.596387 0.325367 11.00000 0.02528 0.08521 = 0.02650 -0.01334 0.00909 -0.00610 N2 5 0.406464 0.703244 0.200701 11.00000 0.06123 0.03647 = 0.01572 0.00268 0.00629 0.01900 N3 5 0.309714 0.543865 0.334519 11.00000 0.03093 0.04967 = 0.01723 0.00189 0.00425 -0.01881 N4 5 0.499881 0.667127 0.419029 11.00000 0.02316 0.02908 = 0.02125 -0.00340 0.00317 0.00048 C1 1 -0.002132 0.628409 0.409521 11.00000 0.01228 0.12965 = 0.04170 -0.04348 0.00619 -0.00421 AFIX 23 H1A 2 -0.106452 0.621290 0.420714 11.00000 -1.20000 H1B 2 0.052807 0.626438 0.491648 11.00000 -1.20000 AFIX 0 C2 1 0.005165 0.671986 0.365617 11.00000 0.01656 0.13765 = 0.04782 -0.04715 -0.00402 0.01815 AFIX 23 H2A 2 -0.066562 0.675914 0.293320 11.00000 -1.20000 H2B 2 -0.022013 0.691531 0.431820 11.00000 -1.20000 AFIX 0 C3 1 0.155984 0.721214 0.263393 11.00000 0.05928 0.07769 = 0.03839 -0.01464 -0.00759 0.04234 AFIX 23 H3A 2 0.099643 0.743257 0.304827 11.00000 -1.20000 H3B 2 0.110705 0.717328 0.178222 11.00000 -1.20000 AFIX 0 C4 1 0.312633 0.734596 0.259035 11.00000 0.07323 0.04710 = 0.02818 -0.00052 -0.00534 0.03373 AFIX 23 H4A 2 0.315735 0.761566 0.212634 11.00000 -1.20000 H4B 2 0.354208 0.740006 0.344622 11.00000 -1.20000 AFIX 0 C5 1 0.377655 0.705348 0.064981 11.00000 0.08569 0.04208 = 0.02025 0.00649 0.00391 0.01972 AFIX 23 H5A 2 0.383015 0.735294 0.038579 11.00000 -1.20000 H5B 2 0.276054 0.695224 0.043005 11.00000 -1.20000 AFIX 0 C6 1 0.483312 0.679675 -0.005690 11.00000 0.06983 0.03588 = 0.01850 0.00358 0.00804 0.00718 AFIX 23 H6A 2 0.445896 0.677323 -0.093592 11.00000 -1.20000 H6B 2 0.580791 0.693790 -0.002386 11.00000 -1.20000 AFIX 0 C7 1 0.585375 0.612377 -0.024460 11.00000 0.03128 0.03522 = 0.02199 -0.00119 0.00701 -0.00299 AFIX 23 H7A 2 0.685671 0.624471 -0.026633 11.00000 -1.20000 H7B 2 0.540740 0.610700 -0.110470 11.00000 -1.20000 AFIX 0 C8 1 0.593767 0.568783 0.032648 11.00000 0.02476 0.03562 = 0.02215 -0.00166 0.00450 -0.00109 AFIX 23 H8A 2 0.633078 0.548805 -0.027364 11.00000 -1.20000 H8B 2 0.664046 0.569479 0.106826 11.00000 -1.20000 AFIX 0 C9 1 0.350267 0.548980 -0.034710 11.00000 0.02866 0.03220 = 0.02164 -0.00193 0.00155 -0.00203 AFIX 23 H9A 2 0.381907 0.526563 -0.091043 11.00000 -1.20000 H9B 2 0.341466 0.575903 -0.081532 11.00000 -1.20000 AFIX 0 C10 1 0.204464 0.537528 0.013211 11.00000 0.03184 0.03699 = 0.02321 -0.00624 0.00230 -0.00758 AFIX 23 H10A 2 0.130550 0.532798 -0.057106 11.00000 -1.20000 H10B 2 0.214384 0.511015 0.061921 11.00000 -1.20000 AFIX 0 C11 1 0.008222 0.564714 0.115780 11.00000 0.02734 0.07351 = 0.02955 -0.01409 0.00500 -0.00877 AFIX 23 H11A 2 -0.004348 0.536421 0.153021 11.00000 -1.20000 H11B 2 -0.057175 0.566579 0.038821 11.00000 -1.20000 AFIX 0 C12 1 -0.030645 0.598810 0.205284 11.00000 0.02682 0.07982 = 0.02887 -0.01390 0.00352 -0.00109 AFIX 23 H12A 2 -0.015479 0.626849 0.167273 11.00000 -1.20000 H12B 2 -0.136407 0.596335 0.220664 11.00000 -1.20000 AFIX 0 C13 1 0.055284 0.553715 0.381703 11.00000 0.02430 0.09945 = 0.02776 0.00144 0.00362 -0.02916 AFIX 23 H13A 2 -0.039699 0.540061 0.354797 11.00000 -1.20000 H13B 2 0.058622 0.556876 0.472883 11.00000 -1.20000 AFIX 0 C14 1 0.179230 0.524810 0.349752 11.00000 0.03354 0.07826 = 0.01735 0.00395 0.00282 -0.02313 C15 1 0.169043 0.481017 0.349032 11.00000 0.05295 0.07875 = 0.02921 0.01453 0.00308 -0.04050 AFIX 43 H15 2 0.075952 0.467741 0.354717 11.00000 -1.20000 AFIX 0 C16 1 0.293188 0.456822 0.340124 11.00000 0.04498 0.05767 = 0.04103 0.01291 0.00345 -0.02490 AFIX 43 H16 2 0.286542 0.426797 0.339840 11.00000 -1.20000 AFIX 0 C17 1 0.428594 0.476529 0.331527 11.00000 0.04432 0.04406 = 0.03058 0.00955 -0.00260 -0.01298 AFIX 43 H17 2 0.516684 0.460514 0.327910 11.00000 -1.20000 AFIX 0 C18 1 0.430749 0.520362 0.328410 11.00000 0.02771 0.03866 = 0.02042 0.00582 -0.00048 -0.00717 C19 1 0.571999 0.545635 0.321930 11.00000 0.02917 0.03598 = 0.01684 0.00865 -0.00447 -0.00722 C20 1 0.561396 0.709119 0.242521 11.00000 0.05249 0.03146 = 0.02962 -0.00060 0.01355 -0.00580 AFIX 23 H20A 2 0.589797 0.739030 0.230560 11.00000 -1.20000 H20B 2 0.623843 0.691134 0.192568 11.00000 -1.20000 AFIX 0 C21 1 0.586729 0.697503 0.377554 11.00000 0.02568 0.02615 = 0.02391 0.00045 0.00547 0.00508 C22 1 0.695801 0.716923 0.455242 11.00000 0.02908 0.02535 = 0.03816 -0.00013 0.01399 0.00628 AFIX 43 H22 2 0.755658 0.738687 0.424736 11.00000 -1.20000 AFIX 0 C23 1 0.715167 0.704058 0.576463 11.00000 0.02232 0.03170 = 0.03844 -0.00645 0.00242 0.00379 AFIX 43 H23 2 0.791493 0.716165 0.629697 11.00000 -1.20000 AFIX 0 C24 1 0.624254 0.673665 0.621004 11.00000 0.02564 0.03282 = 0.02530 0.00080 0.00226 0.00553 AFIX 43 H24 2 0.634907 0.664835 0.705088 11.00000 -1.20000 AFIX 0 C25 1 0.516512 0.656359 0.538919 11.00000 0.02275 0.02842 = 0.02077 -0.00238 0.00047 0.00193 C26 1 0.405007 0.624915 0.579154 11.00000 0.03119 0.03899 = 0.02095 -0.00338 0.00604 -0.00689 SAME 0.02 0.04 F1A > C27A PART 1 F1 4 1.137587 0.636201 0.884398 21.00000 0.06664 0.09772 = 0.06387 -0.00508 -0.01531 0.05507 F2 4 0.931075 0.618752 0.795886 21.00000 0.09358 0.06216 = 0.11295 -0.05393 -0.01861 0.00940 F3 4 1.055945 0.669527 0.721069 21.00000 0.07498 0.11720 = 0.03878 -0.01347 0.01165 0.02649 O9 6 0.870864 0.710552 0.844635 21.00000 0.08682 0.04433 = 0.04661 0.00411 0.00254 0.03574 O10 6 0.936426 0.677706 1.018126 21.00000 0.08422 0.07694 = 0.02783 -0.00199 0.00364 0.01965 C1B 1 1.016463 0.652192 0.826769 21.00000 0.04818 0.05406 = 0.03858 -0.01313 -0.00993 0.02019 C27 1 0.932732 0.683383 0.906587 21.00000 0.01968 0.02595 = 0.03243 0.00067 -0.00200 -0.00213 PART 0 PART 2 F1A 4 1.159141 0.646552 0.864007 -21.00000 0.06125 0.13179 = 0.05699 -0.01141 -0.00605 0.05739 F2A 4 0.952294 0.611800 0.840217 -21.00000 0.10548 0.05645 = 0.07509 -0.02807 -0.03013 0.03459 F3A 4 1.006137 0.656686 0.707385 -21.00000 0.10800 0.13349 = 0.02666 -0.01152 -0.00416 0.08727 O9A 6 0.818560 0.693238 0.857238 -21.00000 0.04694 0.05433 = 0.04110 -0.02098 -0.01070 0.01885 O10A 6 1.004405 0.696239 1.000268 -21.00000 0.06806 0.12606 = 0.05244 -0.04980 -0.01458 0.02621 C1D 1 1.016084 0.649650 0.829444 -21.00000 0.06535 0.06646 = 0.03035 -0.01040 -0.01382 0.03886 C27A 1 0.939119 0.683943 0.904318 -21.00000 0.04094 0.04265 = 0.02910 -0.00434 -0.00088 0.01134 PART 0 AFIX 6 O11 6 0.164494 0.549461 0.690257 11.00000 0.03292 0.04370 = 0.04924 0.00022 0.00252 -0.00254 H11C 2 0.221298 0.527271 0.692349 11.00000 -1.50000 H11D 2 0.225101 0.570801 0.697381 11.00000 -1.50000 AFIX 0 HKLF 4 REM rah14_abs_a.res in P2(1)/c REM R1 = 0.0374 for 5426 Fo > 4sig(Fo) and 0.0384 for all 5604 data REM 491 parameters refined using 351 restraints END WGHT 0.0000 17.7019 REM Highest difference peak 0.873, deepest hole -0.833, 1-sigma level 0.112 Q1 1 0.3339 0.6395 0.2630 11.00000 0.05 0.87 Q2 1 0.3593 0.5997 0.2391 11.00000 0.05 0.83 Q3 1 0.3582 0.6195 0.2017 11.00000 0.05 0.70 Q4 1 0.3070 0.6193 0.4035 11.00000 0.05 0.69 Q5 1 0.4047 0.6190 0.3291 11.00000 0.05 0.60 Q6 1 0.9023 0.6998 0.9795 11.00000 0.05 0.54 Q7 1 0.7253 0.6597 0.2402 11.00000 0.05 0.50 Q8 1 -0.0467 0.6240 0.0724 11.00000 0.05 0.49 Q9 1 0.2770 0.5927 0.3278 11.00000 0.05 0.48 Q10 1 0.2312 0.6424 0.3373 11.00000 0.05 0.48 Q11 1 0.6102 0.6460 0.1746 11.00000 0.05 0.45 Q12 1 0.0588 0.6285 0.4636 11.00000 0.05 0.43 Q13 1 0.4799 0.5736 0.2740 11.00000 0.05 0.41 Q14 1 -0.0650 0.6222 0.1617 11.00000 0.05 0.41 Q15 1 1.1198 0.6658 0.7962 11.00000 0.05 0.40 Q16 1 0.3214 0.5784 0.2939 11.00000 0.05 0.40 Q17 1 0.2109 0.7242 0.4313 11.00000 0.05 0.39 Q18 1 0.4067 0.6637 0.3355 11.00000 0.05 0.39 Q19 1 -0.1839 0.5765 0.4328 11.00000 0.05 0.38 Q20 1 0.4195 0.6409 0.3729 11.00000 0.05 0.38 Q21 1 0.6647 0.5821 0.2163 11.00000 0.05 0.37 Q22 1 0.1270 0.6403 0.3885 11.00000 0.05 0.36 Q23 1 0.3812 0.5379 0.4863 11.00000 0.05 0.36 Q24 1 -0.1805 0.6949 0.1831 11.00000 0.05 0.35 Q25 1 0.1236 0.5663 0.2954 11.00000 0.05 0.35 Q26 1 0.2047 0.5774 0.1373 11.00000 0.05 0.34 Q27 1 0.1713 0.4998 0.3965 11.00000 0.05 0.34 Q28 1 0.3626 0.7244 0.4048 11.00000 0.05 0.34 Q29 1 1.0551 0.6190 0.7975 11.00000 0.05 0.34 Q30 1 0.0416 0.6083 0.1572 11.00000 0.05 0.34 Q31 1 0.6624 0.6094 0.4636 11.00000 0.05 0.33 Q32 1 0.1518 0.6687 0.2409 11.00000 0.05 0.33 Q33 1 -0.0654 0.6169 0.4058 11.00000 0.05 0.33 Q34 1 0.4318 0.6430 0.2474 11.00000 0.05 0.33 Q35 1 0.3950 0.6803 0.0064 11.00000 0.05 0.32 Q36 1 0.4013 0.5830 0.3540 11.00000 0.05 0.32 Q37 1 0.3467 0.7343 0.4327 11.00000 0.05 0.32 Q38 1 0.6365 0.7384 0.1915 11.00000 0.05 0.32 Q39 1 0.5367 0.6776 0.4649 11.00000 0.05 0.32 Q40 1 0.3063 0.5580 0.1771 11.00000 0.05 0.32 ; _shelx_res_checksum 52177 _shelx_hkl_file ; 0 0 -1 1.17 0.67 0 0 -1 -2.22 3.32 0 0 -2 4299.78 225.78 0 0 -2 3918.93 234.52 0 0 -3 8.82 2.44 0 0 -3 2.01 7.32 0 0 -4 246.00 27.25 0 0 -4 299.77 18.60 0 0 -4 256.27 28.22 0 0 -4 208.42 17.24 0 0 -4 186.32 25.04 0 0 -5 11.88 10.80 0 0 -5 9.59 8.50 0 0 -5 7.27 4.87 0 0 -5 3.08 5.80 0 0 -5 9.27 4.63 0 0 -6 747.66 45.12 0 0 -6 833.16 65.82 0 0 -6 729.80 63.16 0 0 -7 2.53 2.54 0 0 -7 5.49 2.69 0 0 -7 13.76 10.55 0 0 -7 2.29 3.89 0 0 -7 8.95 9.40 0 0 -7 7.86 4.84 0 0 -7 6.61 3.05 0 0 -7 0.58 2.34 0 0 -7 6.77 4.86 0 0 -7 9.61 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110.59 8.02 0 -28 -9 123.58 9.25 0 28 -9 116.83 9.43 0 29 0 -0.75 2.80 0 29 -1 103.36 10.37 0 -29 -1 92.52 20.20 0 -29 1 116.82 11.50 0 -29 -1 120.20 11.72 0 -29 -2 47.74 6.55 0 -29 2 51.78 7.53 0 -29 -2 51.97 7.54 0 29 -2 68.49 9.13 0 29 -2 54.04 6.59 0 -29 -2 51.47 16.06 0 -29 -3 208.87 30.67 0 -29 -3 253.56 18.12 0 29 -3 240.15 19.85 0 -29 3 246.24 18.54 0 29 -3 238.60 16.80 0 -29 -4 53.12 7.19 0 29 -4 47.14 6.09 0 -29 4 59.30 7.17 0 -29 -4 41.72 6.21 0 -29 -4 59.22 14.85 0 29 -5 427.78 30.30 0 -29 5 449.49 28.24 0 -29 -5 410.69 27.67 0 29 -5 470.21 28.17 0 -29 -5 455.42 28.89 0 29 -6 174.35 13.39 0 29 -6 171.53 12.35 0 -29 6 133.45 11.12 0 29 -6 134.99 10.67 0 29 -7 215.10 15.10 0 29 -7 211.17 15.85 0 29 -7 231.18 16.79 0 29 -7 205.55 14.06 0 29 7 212.41 15.27 0 29 -8 22.37 3.88 0 29 -8 18.10 3.29 0 29 -8 19.76 3.66 0 29 8 21.55 3.15 0 29 -8 18.97 2.72 0 -29 -9 39.06 4.21 0 29 -9 30.47 4.02 0 30 0 604.54 37.78 0 30 1 35.69 5.80 0 30 -1 28.67 5.18 0 -30 -1 37.64 6.30 0 -30 1 30.65 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1637.20 92.22 1 -2 -9 1612.48 88.83 1 -2 -9 1508.70 88.21 1 -2 -9 1613.81 94.34 1 2 -9 1494.45 88.36 1 2 -9 1663.96 91.69 1 -2 -9 1616.81 91.24 1 2 -9 1692.85 91.56 1 2 -9 1551.63 89.76 1 -2 -9 1518.34 89.35 1 2 -9 1677.50 91.10 1 2 -9 1556.32 88.17 1 -2 -9 1568.19 92.39 1 -2 -8 4.86 3.87 1 2 -8 3.20 2.48 1 -2 -8 -1.23 4.63 1 -2 -8 2.16 3.10 1 -2 -8 1.86 2.47 1 -2 -8 3.35 3.05 1 2 -8 2.62 2.96 1 2 -8 4.72 3.13 1 -2 -8 -0.77 2.81 1 -2 -8 5.88 2.88 1 2 -8 5.70 2.92 1 2 -8 1.64 3.09 1 2 -8 3.58 2.81 1 -2 -8 7.77 3.98 1 -2 -8 3.36 2.53 1 -2 -8 2.12 3.98 1 -2 -8 10.58 4.19 1 2 -8 1.50 2.54 1 -2 -8 4.26 2.74 1 2 -8 1.24 4.35 1 -2 -7 1910.99 116.31 1 2 -7 1970.53 117.13 1 -2 -7 2103.28 114.42 1 2 -7 2001.17 114.10 1 -2 -7 2025.59 112.97 1 2 -7 2085.06 114.15 1 -2 -7 2313.56 143.52 1 -2 -7 2082.80 113.47 1 2 -7 1967.33 113.22 1 -2 -7 2028.15 113.13 1 -2 -7 2261.46 118.46 1 2 -7 2090.49 114.92 1 -2 -7 2088.81 114.58 1 2 -7 2065.28 114.11 1 -2 -7 2132.28 113.61 1 2 -7 2090.31 114.86 1 2 -7 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26 -5 64.07 7.82 2 -26 -5 72.77 7.45 2 -26 -5 79.14 7.52 2 -26 -5 73.45 8.32 2 26 -5 60.69 9.79 2 26 -5 61.65 6.96 2 26 -4 421.23 28.78 2 26 -4 464.85 28.62 2 -26 -4 384.32 42.14 2 -26 -4 420.88 27.17 2 -26 -4 443.46 27.09 -2 -26 4 448.73 28.57 2 26 -4 471.46 31.62 2 -26 -4 384.38 27.31 2 26 -4 416.29 26.89 2 -26 -4 478.83 29.46 2 -26 -3 167.74 25.29 2 26 -3 160.52 13.76 2 26 -3 163.12 15.57 -2 -26 3 166.52 14.13 2 -26 -3 163.48 13.48 2 26 -2 413.33 28.53 -2 -26 2 397.65 41.69 -2 -26 2 440.04 29.00 2 -26 -2 415.75 28.02 2 26 -2 461.87 30.52 -2 -26 1 6.68 7.72 2 26 -1 14.47 4.21 2 26 -1 19.10 5.04 -2 -26 1 14.71 4.41 2 -26 -1 17.47 4.29 -2 -26 0 292.39 19.62 2 26 0 330.03 22.45 -2 -26 0 270.84 34.53 2 -26 0 280.51 21.07 -2 -26 -1 -3.70 7.76 2 26 1 2.51 3.23 -2 -26 -1 1.70 1.76 -2 -26 -2 4.96 2.79 -2 -26 -2 -1.28 2.56 2 -26 2 6.74 3.30 -2 -26 -2 -3.86 6.28 -2 -26 -3 3.46 2.49 -2 -26 -3 1.99 2.65 -2 -26 -3 6.85 3.60 2 -26 3 5.21 3.50 2 26 3 5.86 4.23 -2 -26 -3 4.03 8.45 -2 -26 -4 81.74 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21.59 4.00 5 27 5 26.93 4.47 -5 27 -6 13.43 2.26 5 -27 6 13.16 2.72 -5 -27 -6 16.75 3.02 5 27 6 15.42 3.15 5 27 6 14.27 2.73 5 27 7 22.64 3.07 -5 -27 -7 18.43 3.03 -5 -27 -7 14.20 2.56 -5 27 -7 14.72 2.34 5 -27 7 12.93 2.03 5 28 -8 9.97 1.96 5 28 -8 10.10 1.94 5 -28 -7 115.73 8.03 5 28 -7 104.47 8.98 5 28 -7 119.95 9.49 5 28 -7 105.41 8.77 5 -28 -6 45.26 5.63 -5 -28 6 42.77 4.97 5 -28 -6 48.53 4.95 5 28 -6 51.94 5.94 5 -28 -5 317.22 21.69 5 -28 -5 326.46 20.32 5 28 -5 316.34 21.54 5 28 -4 21.99 4.41 5 -28 -4 22.71 4.84 5 28 -4 24.69 4.60 5 -28 -4 29.07 4.21 5 28 -3 356.29 24.78 -5 -28 3 392.23 24.65 5 -28 -3 409.70 26.30 5 28 -3 372.28 25.70 -5 -28 2 24.02 5.08 5 -28 -2 14.68 3.37 -5 -28 2 19.32 4.35 5 28 -2 17.68 3.76 5 28 -2 22.56 4.60 5 -28 -1 192.02 14.31 -5 -28 1 183.95 15.19 -5 -28 1 222.40 16.12 5 28 -1 166.56 14.14 5 28 -1 190.07 15.39 -5 -28 0 1.45 2.89 5 -28 0 4.77 2.75 -5 -28 0 -0.78 3.19 -5 -28 0 1.53 2.97 5 28 0 3.93 3.69 -5 -28 -1 23.96 4.70 -5 -28 -1 30.61 5.64 -5 -28 -1 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177.78 12.67 7 25 -5 170.13 11.93 7 25 -5 186.47 13.72 7 25 -5 207.86 13.61 7 25 -4 47.21 6.15 7 25 -4 36.00 4.65 -7 -25 4 56.95 6.25 -7 -25 4 54.37 6.27 7 -25 -4 49.96 6.36 7 25 -4 51.55 5.70 7 25 -4 52.04 6.67 7 -25 -4 50.72 5.22 -7 -25 3 231.97 16.75 -7 -25 3 249.26 16.86 7 -25 -3 236.49 16.98 7 25 -3 221.08 16.02 7 -25 -3 217.54 14.93 7 25 -3 208.31 16.85 -7 -25 2 29.23 5.13 -7 -25 2 25.28 4.71 7 -25 -2 13.66 3.88 7 25 -2 15.51 3.94 7 -25 -2 18.78 3.15 7 25 -2 22.47 4.35 7 25 -1 320.31 23.53 7 25 -1 322.58 22.79 -7 -25 1 343.71 22.77 -7 -25 1 353.49 23.15 7 25 -1 309.83 22.11 7 25 0 35.61 5.73 -7 -25 0 40.81 6.07 7 25 0 33.27 6.12 7 -25 0 28.23 4.40 7 25 0 40.77 6.32 7 25 1 164.02 13.37 7 25 1 136.15 10.66 -7 -25 -1 132.17 10.14 -7 25 -1 129.40 10.61 -7 -25 -2 6.39 3.05 7 25 2 6.17 3.42 -7 -25 -2 2.96 3.01 7 25 2 3.74 2.12 7 25 2 6.93 3.75 -7 -25 -2 4.47 2.04 -7 25 -2 13.06 3.38 -7 -25 -3 22.26 3.43 7 25 3 19.99 4.10 -7 -25 -3 20.25 3.76 7 25 3 24.70 3.91 7 25 3 28.01 4.99 7 25 4 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128.84 13.47 8 15 -2 110.41 12.96 8 15 -2 118.44 13.60 8 15 -2 115.98 10.93 8 15 -2 113.22 11.73 -8 15 2 122.34 10.55 8 -15 -2 109.66 10.85 8 -15 -2 139.33 11.97 8 15 -2 118.54 12.81 -8 15 1 6.82 3.22 8 -15 -1 2.27 2.49 8 15 -1 9.36 6.02 -8 -15 1 5.57 4.68 8 15 -1 3.58 2.79 8 -15 -1 5.63 3.48 -8 -15 1 13.43 5.58 8 15 -1 9.51 4.30 8 15 -1 10.43 5.23 8 15 -1 13.84 4.83 8 15 -1 8.68 4.95 -8 -15 0 663.00 40.03 -8 -15 0 540.50 38.86 8 15 0 649.54 40.78 8 15 0 568.03 38.95 8 15 0 487.79 38.09 -8 15 0 586.15 36.53 8 15 0 590.52 37.77 -8 -15 -1 21.17 6.24 -8 -15 -1 25.17 6.47 8 15 1 11.26 6.16 8 15 1 11.14 4.97 8 15 1 34.66 7.73 8 15 1 23.01 6.35 -8 15 -1 10.17 4.10 8 15 1 10.49 4.06 -8 -15 -2 479.17 33.58 -8 -15 -2 450.24 32.94 -8 15 -2 457.02 31.26 8 15 2 551.14 34.90 8 15 2 465.64 32.50 8 15 3 2.06 3.88 8 15 3 4.61 4.84 8 15 3 6.80 3.33 -8 15 -3 3.49 3.01 -8 15 -3 7.65 4.38 -8 -15 -4 392.88 27.55 8 15 4 504.70 31.17 8 15 4 504.66 32.59 -8 -15 -4 442.44 30.16 -8 15 -5 17.80 4.88 8 15 5 10.35 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445.77 28.68 10 -5 -1 408.71 28.54 -10 -5 1 374.09 24.08 10 -5 -1 367.26 27.64 10 5 -1 405.50 28.07 -10 5 1 404.37 24.82 -10 -5 1 431.33 25.85 10 5 -1 360.19 24.07 -10 5 0 246.88 17.48 -10 -5 0 272.23 18.15 -10 -5 0 243.85 17.07 10 5 1 175.49 13.89 -10 5 -1 162.00 12.87 -10 -5 -1 170.00 13.46 -10 -5 -1 171.37 12.96 10 5 2 72.63 7.92 10 5 2 63.70 7.42 -10 5 -2 69.95 7.40 -10 -5 -2 62.20 7.11 10 5 3 14.87 3.61 10 5 3 19.42 3.97 -10 -5 -3 18.83 3.98 -10 -5 -3 19.40 4.10 -10 -5 -4 25.93 4.35 -10 5 -4 19.18 3.85 -10 -5 -4 16.40 3.50 -10 5 -4 22.91 4.85 -10 -5 -4 16.48 4.49 -10 5 -5 11.32 2.75 -10 5 -5 20.14 3.60 -10 -5 -5 16.38 3.36 10 -6 -7 440.28 25.55 10 6 -6 16.34 2.86 10 -6 -6 23.49 3.63 10 -6 -6 19.62 3.47 10 6 -5 342.43 21.83 10 -6 -5 364.95 22.74 10 -6 -5 349.64 23.13 10 6 -4 19.86 4.83 10 -6 -4 27.64 5.55 10 6 -4 17.83 3.62 10 6 -4 24.51 5.13 10 -6 -4 14.25 4.41 -10 -6 4 17.78 3.13 10 -6 -4 24.50 4.99 10 6 -4 26.70 5.27 10 6 -3 38.92 6.40 10 -6 -3 36.13 6.82 10 6 -3 37.42 5.06 10 6 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330.04 22.31 10 9 -3 336.37 22.02 10 -9 -3 345.84 21.59 10 9 -3 296.27 21.68 10 -9 -3 279.09 21.40 10 -9 -2 81.55 7.78 10 -9 -2 71.70 8.31 10 9 -2 57.08 7.33 10 9 -2 66.44 7.43 10 -9 -2 52.26 6.95 -10 9 2 73.77 6.37 10 -9 -2 55.58 7.35 10 9 -2 47.68 6.94 -10 -9 2 61.41 7.07 10 -9 -1 302.23 23.94 10 9 -1 361.28 24.56 -10 9 1 375.42 23.11 -10 -9 1 439.10 25.15 10 9 -1 366.35 24.53 10 -9 -1 328.05 24.43 10 9 -1 358.83 24.26 -10 -9 1 404.78 23.51 10 9 0 61.70 8.44 10 9 0 56.95 7.83 -10 9 0 88.84 7.73 10 -9 0 53.78 7.55 10 9 0 57.24 7.73 -10 -9 0 80.74 8.27 10 9 0 66.40 8.05 10 -9 0 72.32 8.58 10 9 0 68.16 7.48 -10 -9 0 74.24 7.47 10 9 1 178.51 14.47 10 9 1 157.52 14.54 -10 9 -1 188.51 13.28 10 9 1 148.10 12.57 -10 -9 -1 185.54 13.51 10 9 2 83.35 9.11 -10 9 -2 60.38 7.17 -10 -9 -2 61.96 7.68 -10 -9 -2 84.14 8.25 10 9 3 13.58 3.90 10 9 3 9.36 3.43 -10 9 -3 15.00 3.56 -10 -9 -3 10.46 3.14 -10 9 -3 18.20 3.73 -10 -9 -3 11.37 3.24 -10 -9 -3 11.27 3.48 10 9 4 30.79 4.29 10 9 4 34.70 5.00 -10 9 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248.26 19.17 -10 11 0 301.69 18.66 -10 -11 0 327.31 20.51 10 -11 0 266.40 17.95 10 -11 1 63.21 7.00 -10 -11 -1 77.52 7.88 10 11 1 51.99 6.98 10 11 1 66.90 8.12 10 11 1 66.86 8.45 -10 11 -1 80.33 7.55 10 -11 1 55.87 5.93 -10 -11 -2 70.45 7.18 10 11 2 33.43 5.11 10 11 2 50.97 7.25 10 11 2 42.13 6.52 -10 11 -2 59.48 6.17 -10 11 -2 62.81 6.55 -10 -11 -2 47.75 5.97 -10 -11 -3 28.27 4.96 -10 11 -3 23.39 3.47 10 11 3 20.32 4.72 -10 11 -3 31.20 4.75 -10 -11 -3 26.48 3.75 10 11 4 3.46 2.07 10 11 4 -0.42 1.78 10 -12 -6 148.69 9.62 10 -12 -5 62.77 5.10 10 12 -5 44.18 5.58 10 -12 -4 101.18 7.40 -10 -12 4 83.59 7.50 10 -12 -4 81.06 8.00 10 12 -4 73.02 8.12 10 -12 -3 13.27 2.93 -10 -12 3 21.39 4.36 10 -12 -3 18.85 4.29 10 -12 -3 14.55 3.39 10 12 -3 7.65 3.52 10 -12 -2 3.00 2.41 10 -12 -2 0.96 2.35 10 12 -2 0.69 2.82 10 -12 -2 3.79 2.54 -10 -12 2 3.97 3.11 10 -12 -1 17.97 3.90 -10 -12 1 18.15 3.77 10 12 -1 12.74 4.21 10 -12 -1 20.94 4.08 -10 12 1 18.62 3.50 -10 -12 1 21.67 4.83 10 -12 0 28.97 4.52 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15.96 10 13 -1 225.32 17.77 -10 -13 1 282.29 17.61 10 13 0 9.76 3.64 -10 13 0 8.83 2.91 10 -13 0 5.36 2.59 10 -13 0 1.62 2.85 -10 -13 0 7.79 3.10 10 13 0 13.25 3.90 -10 13 -1 161.81 12.03 -10 -13 -1 143.54 12.03 10 13 1 193.92 12.93 10 -13 1 145.16 10.75 10 13 1 115.87 11.65 -10 -13 -1 166.46 12.64 -10 13 -2 13.08 3.54 -10 -13 -2 16.41 3.36 10 13 2 26.37 4.74 10 13 2 20.20 4.03 -10 -13 -2 16.53 3.81 10 13 2 12.18 3.13 -10 13 -3 31.56 4.18 -10 -13 -3 26.65 3.22 10 13 3 28.90 4.32 -10 -13 -3 30.39 4.22 10 13 4 16.48 2.70 10 -14 -5 100.09 7.35 10 14 -5 94.61 7.75 10 -14 -4 33.83 3.59 -10 -14 4 36.35 4.05 10 -14 -4 28.53 4.08 10 14 -4 27.45 4.39 10 -14 -3 18.04 2.87 -10 -14 3 12.80 3.48 10 -14 -3 9.50 2.82 10 14 -3 20.39 4.28 10 -14 -2 10.07 2.61 -10 -14 2 14.61 4.03 10 -14 -2 8.84 3.24 10 14 -2 7.70 3.89 10 -14 -1 23.52 3.49 -10 -14 1 19.14 4.31 10 -14 -1 12.65 3.07 -10 -14 1 17.52 3.75 10 14 -1 28.79 4.98 -10 14 0 28.21 4.26 10 -14 0 26.99 3.88 -10 -14 0 36.22 5.39 10 14 0 32.69 5.23 -10 14 -1 81.45 7.92 -10 -14 -1 91.90 8.41 10 14 1 109.78 8.54 10 14 1 94.96 8.74 -10 -14 -1 80.65 8.37 -10 14 -2 58.50 6.08 -10 -14 -2 59.60 5.70 10 14 2 62.43 6.29 10 14 2 77.07 6.98 10 14 2 43.21 5.39 -10 -14 -2 48.65 5.98 -10 14 -3 111.80 8.90 10 14 3 130.12 9.29 10 14 3 129.10 9.36 -10 -14 -3 106.42 8.84 10 -15 -5 5.49 1.52 10 15 -5 7.51 1.88 10 -15 -4 194.02 12.36 10 -15 -4 166.93 11.40 10 -15 -4 171.67 11.18 10 -15 -3 20.01 2.79 -10 -15 3 19.01 3.73 10 -15 -3 28.14 3.92 10 15 -3 16.65 3.61 10 -15 -2 330.13 20.05 -10 -15 2 343.87 22.47 10 -15 -2 302.52 20.91 10 15 -2 388.49 22.42 10 -15 -1 15.09 2.71 -10 -15 1 14.95 3.77 10 -15 -1 11.99 2.78 -10 -15 1 9.83 3.03 10 15 -1 17.05 3.71 -10 15 0 201.09 13.07 10 -15 0 162.21 12.20 -10 -15 0 198.76 14.42 -10 15 -1 9.32 2.86 -10 -15 -1 13.32 3.25 10 15 1 15.89 2.91 -10 -15 -1 9.34 3.20 10 15 1 17.26 3.48 -10 15 -2 55.25 5.66 -10 -15 -2 62.07 5.27 10 15 2 64.54 5.71 10 15 2 42.75 4.93 -10 -15 -2 61.84 6.02 -10 15 -3 15.59 2.68 10 15 3 12.46 2.52 10 15 3 16.78 2.63 -10 -15 -3 14.09 2.67 10 -16 -4 54.27 4.72 10 16 -4 51.59 5.06 10 -16 -3 16.53 2.26 -10 -16 3 12.69 3.05 10 -16 -3 23.89 3.24 10 16 -3 19.55 3.43 10 -16 -2 7.34 1.90 -10 -16 2 12.79 3.28 10 -16 -2 11.02 2.48 10 16 -2 16.23 3.29 10 -16 -1 13.83 2.56 -10 -16 1 23.81 4.16 -10 -16 1 15.13 3.06 10 16 -1 18.23 3.69 10 16 0 48.60 5.53 -10 16 0 46.65 4.37 10 -16 0 43.93 4.38 -10 16 -1 80.27 6.49 -10 -16 -1 78.66 6.78 10 16 1 78.26 6.81 10 16 1 62.55 6.58 -10 -16 -1 90.99 7.49 -10 16 -2 117.17 8.62 -10 -16 -2 105.99 7.99 10 16 2 114.94 8.39 10 16 3 56.45 4.83 -10 -16 -3 61.00 4.94 10 17 -4 0.25 1.75 -10 -17 3 282.34 17.30 10 -17 -3 284.52 16.71 10 17 -3 266.29 17.35 -10 -17 2 13.26 2.89 10 -17 -2 16.33 2.35 10 17 -2 11.07 2.87 10 17 -1 278.67 16.38 -10 -17 1 259.74 15.72 -10 -17 1 301.64 16.82 10 -17 0 4.35 1.46 -10 -17 0 9.93 2.43 10 17 0 4.78 2.17 10 17 1 144.86 11.07 -10 -17 -1 168.84 11.22 10 17 2 11.92 2.25 -10 -17 -2 10.97 2.38 10 18 -3 24.27 3.19 -10 -18 2 7.64 2.13 10 18 -2 3.04 2.07 -10 -18 1 10.61 2.40 10 18 -1 5.09 1.90 -10 -18 0 33.81 3.76 -10 -18 0 36.76 3.78 10 18 0 28.06 3.61 -10 -18 -1 48.72 4.40 -10 -18 -1 62.62 5.03 -10 -19 2 170.17 11.30 10 19 -2 185.63 11.43 10 19 -1 2.55 1.42 -10 -19 0 164.33 10.50 11 0 -4 414.21 26.47 11 0 -4 477.97 25.95 11 0 -3 5.73 2.40 11 0 -3 -0.30 1.98 -11 0 2 211.38 13.88 11 0 -2 246.23 14.77 -11 0 1 13.53 2.65 11 0 -1 5.39 2.48 -11 0 0 177.97 11.78 11 0 0 160.67 11.45 -11 0 -1 26.74 3.90 11 0 1 23.10 3.30 -11 0 -2 3.35 2.52 -11 0 -2 -0.33 1.72 -11 0 -3 20.78 3.49 11 -1 -4 14.55 2.84 11 1 -4 8.51 2.32 11 -1 -4 8.36 2.17 11 -1 -3 17.49 3.25 11 -1 -3 12.19 4.09 11 1 -3 15.22 2.61 11 -1 -3 16.21 3.04 11 -1 -2 32.43 6.11 11 1 -2 31.28 3.75 11 -1 -2 41.91 4.51 -11 1 2 33.15 3.45 -11 -1 2 31.41 3.59 11 -1 -1 102.99 10.53 11 1 -1 96.02 7.73 11 -1 -1 107.09 8.47 -11 1 1 105.91 7.84 -11 -1 1 102.35 7.99 11 -1 0 170.54 14.32 11 1 0 160.14 11.08 11 -1 0 148.22 11.50 -11 1 0 192.13 11.88 -11 -1 0 178.16 11.85 11 -1 1 239.33 18.35 11 -1 1 229.01 15.71 -11 1 -1 270.55 16.21 -11 -1 -1 265.58 16.29 11 -1 2 135.01 12.51 -11 1 -2 160.19 12.81 -11 1 -3 115.75 9.15 11 -2 -4 1.10 1.79 11 -2 -4 4.22 1.70 11 -2 -3 417.84 24.17 11 2 -3 393.08 25.34 11 -2 -3 354.70 25.01 11 -2 -3 395.16 23.63 11 2 -2 3.72 3.44 11 -2 -2 7.07 3.99 11 -2 -2 11.71 2.84 -11 -2 2 13.59 2.40 11 2 -1 284.91 19.36 11 -2 -1 243.96 18.89 11 -2 -1 264.57 17.15 -11 2 1 250.69 16.20 -11 -2 1 273.69 16.65 11 2 0 15.44 4.75 11 -2 0 17.00 5.01 11 -2 0 21.51 3.84 -11 2 0 20.14 3.35 -11 -2 0 18.86 3.42 -11 2 -1 19.61 3.01 -11 -2 -1 21.13 3.28 11 2 1 12.48 4.09 11 -2 1 11.55 4.14 11 2 2 32.63 4.82 11 -2 2 16.61 4.13 -11 2 -2 22.82 4.36 -11 2 -2 27.23 3.68 11 -3 -4 10.49 2.45 11 -3 -4 12.31 2.46 11 3 -3 29.40 4.81 11 -3 -3 25.08 4.72 11 -3 -3 24.01 3.69 11 3 -2 67.17 7.51 11 -3 -2 55.96 7.31 11 -3 -2 60.33 6.17 -11 -3 2 61.56 5.34 11 3 -1 96.17 9.09 11 -3 -1 82.79 8.99 11 -3 -1 74.27 7.48 -11 3 1 91.10 6.96 -11 -3 1 84.79 7.15 11 3 0 196.20 14.83 11 -3 0 183.45 14.86 11 -3 0 168.52 13.22 -11 3 0 192.84 12.82 -11 -3 0 218.33 13.38 -11 3 -1 120.10 8.98 -11 -3 -1 124.54 9.21 11 3 1 115.23 10.26 11 -3 1 120.27 10.70 11 3 2 193.28 14.90 11 -3 2 216.35 15.60 -11 3 -2 244.74 15.97 -11 -3 -2 234.15 15.70 -11 3 -2 221.47 14.29 11 -4 -4 311.64 19.16 11 -4 -4 303.83 18.83 11 4 -3 21.39 3.97 11 -4 -3 26.20 4.50 11 -4 -3 26.20 3.71 11 4 -2 172.87 13.51 11 -4 -2 183.51 13.97 11 -4 -2 147.84 12.38 -11 -4 2 182.86 11.88 11 4 -1 10.73 3.87 11 -4 -1 6.39 3.61 11 -4 -1 5.32 2.71 -11 4 1 10.01 2.42 -11 -4 1 15.30 3.08 11 4 0 124.84 11.04 11 -4 0 117.99 10.26 -11 4 0 134.70 9.71 -11 -4 0 147.64 10.24 -11 4 -1 29.63 3.98 -11 -4 -1 34.08 4.36 11 4 1 22.59 4.20 11 -4 1 31.44 5.04 11 4 2 0.39 1.81 11 -4 2 0.45 1.92 -11 4 -2 0.45 1.92 -11 -4 -2 4.02 2.34 -11 4 -2 4.16 1.75 11 -5 -4 7.73 2.18 11 -5 -4 7.43 2.07 11 5 -3 3.71 2.48 11 -5 -3 8.21 3.02 11 -5 -3 11.30 2.59 11 5 -2 63.35 6.70 11 -5 -2 60.59 6.98 11 -5 -2 57.47 6.16 -11 -5 2 68.53 5.74 11 -5 -2 64.43 6.11 11 5 -1 123.28 10.18 11 -5 -1 130.19 10.68 11 -5 -1 118.24 9.82 -11 5 1 112.56 8.54 -11 -5 1 145.46 9.70 11 5 0 62.47 6.75 11 -5 0 78.79 7.57 -11 5 0 63.37 5.74 -11 -5 0 69.53 6.19 -11 5 -1 209.79 14.22 -11 -5 -1 246.36 15.02 11 5 1 212.81 15.04 11 -5 1 222.79 15.51 -11 5 -2 44.53 5.02 -11 -5 -2 38.97 4.80 -11 5 -2 58.51 5.02 -11 -5 -2 52.20 5.09 11 5 2 44.89 4.70 11 -5 2 43.32 4.93 11 -6 -4 5.94 1.86 11 -6 -3 358.14 22.21 -11 -6 2 20.17 3.17 11 -6 -2 26.54 3.74 11 6 -2 18.48 3.56 11 -6 -2 21.21 4.11 -11 -6 1 78.23 6.72 11 -6 -1 79.41 6.60 11 6 -1 65.31 6.74 11 -6 -1 73.31 7.26 -11 6 0 19.28 3.04 -11 -6 0 21.63 3.60 11 -6 0 27.07 3.36 11 6 0 13.78 3.26 11 -6 0 18.35 3.83 -11 6 -1 11.75 2.40 -11 -6 -1 11.07 2.70 11 6 1 11.08 2.53 11 -6 1 9.10 2.96 -11 6 -2 12.78 2.54 -11 -6 -2 9.74 2.34 11 -7 -3 20.97 3.55 -11 -7 2 122.67 9.21 11 7 -2 115.12 9.32 11 -7 -2 128.42 9.93 -11 -7 1 92.27 7.18 11 -7 -1 85.22 6.63 11 -7 -1 75.15 7.12 -11 7 0 162.89 10.77 11 -7 0 162.42 10.71 11 7 0 131.16 10.78 11 -7 0 153.59 11.56 11 -7 1 67.01 5.89 -11 7 -1 52.89 5.50 -11 -7 -1 59.55 5.73 -11 7 -1 62.00 5.44 -11 7 -2 111.18 7.95 -11 -7 -2 103.11 7.85 11 -8 -3 24.18 3.33 11 -8 -3 20.11 2.89 11 -8 -2 295.21 15.92 -11 -8 2 265.81 15.80 11 -8 -2 223.45 15.57 11 -8 -2 212.64 15.46 11 -8 -1 14.84 2.95 -11 -8 1 23.78 3.58 11 -8 -1 20.81 3.05 -11 -8 0 98.18 7.67 11 -8 0 88.03 6.55 -11 8 -1 19.76 2.89 11 -9 -3 22.92 2.74 11 -9 -3 22.01 3.03 11 -9 -2 28.73 3.38 11 -9 -2 20.66 3.11 11 -9 -1 231.55 13.63 11 -9 -1 190.85 13.27 -11 -9 1 213.17 14.22 11 -9 0 36.40 4.03 -11 -9 0 40.72 4.57 11 -9 1 200.57 12.67 11 -10 -2 36.01 3.49 11 -10 -2 29.23 3.44 11 -10 -1 145.76 9.50 -11 -10 1 133.99 10.03 11 -10 0 18.65 2.67 -11 -10 0 23.84 3.31 11 -11 -1 6.69 1.63 -11 -11 1 6.32 1.97 -11 -11 0 114.12 8.21 0 0 0 0.00 0.00 TITL Rah14_abs in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.087195 31.576416 10.820844 90.0000 94.0560 90.0000 ZERR 4.00 0.000069 0.000287 0.000070 0.0000 0.0006 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O F Bi UNIT 112.00 124.00 16.00 44.00 16.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1038 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.324 _oxdiff_exptl_absorpt_empirical_full_min 0.773 #---End data_Bi-py-macrodipa _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Justin J. Wilson' _publ_contact_author_address ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; _publ_contact_author_email jjw275@cornell.edu _publ_contact_author_phone 1(607)2554344 loop_ _publ_author_name _publ_author_address 'Hu, Aohan' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; 'Brown, Victoria' ;Department of Chemistry Simon Fraser University Burnaby, British Columbia V5A 1S6 Canada ; 'MacMillan, Samantha N.' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; 'Radchenko, Valery' ;Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada Department of Chemistry University of British Columbia Vancouver, British Columbia V6T 1Z1 Canada ; 'Yang, Hua' ;Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Wharton, Luke' ;Department of Chemistry University of British Columbia Vancouver, British Columbia V6T 1Z1 Canada Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Ramogida, Caterina F.' ;Department of Chemistry Simon Fraser University Burnaby, British Columbia V5A 1S6 Canada Life Sciences Division TRIUMF Vancouver, British Columbia V6T 2A3 Canada ; 'Wilson, Justin J.' ;Department of Chemistry and Chemical Biology Cornell University Ithaca, New York 14853 United States ; _audit_creation_date 2020-12-04 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032) ; _shelx_SHELXL_version_number '2016/6' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C29 H33 Bi N5 O7, C2 F3 O2, C3 H7 N O, O' _chemical_formula_sum 'C34 H40 Bi F3 N6 O11' _chemical_formula_weight 974.70 _chemical_melting_point ? _chemical_oxdiff_formula C34B40BiF3N6O10 _chemical_oxdiff_usercomment 'Crystallized from DMF/ether.' 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' 'Bi' 'Bi' -4.1077 10.2566 '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' _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/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3865(3) _cell_length_b 12.6811(2) _cell_length_c 21.5862(4) _cell_angle_alpha 90 _cell_angle_beta 91.723(2) _cell_angle_gamma 90 _cell_volume 3662.72(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 17958 _cell_measurement_temperature 100.0(3) _cell_measurement_theta_max 31.9480 _cell_measurement_theta_min 2.4720 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 4.898 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1936 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 17 -1 10 0.0187 -18 1 -10 0.0299 17 7 5 0.0574 -1 -17 10 0.1621 -6 11 22 0.0958 -6 1 29 0.0369 6 -1 -29 0.0240 3 12 -21 0.0932 7 -1 28 0.0279 -7 1 -28 0.0249 18 -2 -9 0.0130 -18 0 10 0.0309 _exptl_crystal_size_max 0.325 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.051 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 17.4797 -1.0681 10.4374 0.9603 -0.2303 -0.1573 -17.5571 0.6559 -10.2109 -0.9638 0.2311 0.1330 17.1568 6.5046 5.3041 0.9283 -0.2225 0.2979 -0.9430 -16.7803 10.4509 -0.0200 0.0046 -0.9998 -5.7551 10.9507 22.4684 -0.2216 -0.9244 0.3106 -6.1170 0.5609 29.0688 -0.2217 -0.9246 -0.3097 6.1591 -1.1457 -28.9969 0.2240 0.9340 0.2783 3.2637 12.3956 -21.4540 0.1026 0.4270 0.8984 6.5204 -1.1140 28.1687 0.4427 -0.8149 -0.3741 -6.5002 1.2227 -28.1688 -0.4416 0.8129 0.3798 18.0584 -2.4225 -8.6579 0.9237 0.3829 -0.0091 -17.9656 -0.1111 10.1651 -0.9146 -0.3792 -0.1408 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 44156 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 2.460 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(3) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -32.00 16.00 0.50 10.10 -- 4.12 -57.00 -60.00 96 2 \w -15.00 26.00 0.50 10.10 -- -4.74 -99.00-120.00 82 3 \w -67.00 -7.00 0.50 10.10 -- 4.12 -27.00 9.00 120 4 \w 3.00 34.00 0.50 10.10 -- 4.12 -99.00 60.00 62 5 \w -9.00 23.00 0.50 10.10 -- 4.12 -99.00 150.00 64 6 \w 9.00 35.00 0.50 10.10 -- 4.12 27.00 172.00 52 7 \w -75.00 7.00 0.50 10.10 -- -4.74 -57.00-150.00 164 8 \w -22.00 9.00 0.50 10.10 -- 4.12 95.00 166.13 62 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0528788000 _diffrn_orient_matrix_UB_12 0.0003936000 _diffrn_orient_matrix_UB_13 0.0034914000 _diffrn_orient_matrix_UB_21 0.0039075000 _diffrn_orient_matrix_UB_22 -0.0195580000 _diffrn_orient_matrix_UB_23 -0.0306079000 _diffrn_orient_matrix_UB_31 0.0010373000 _diffrn_orient_matrix_UB_32 0.0523932000 _diffrn_orient_matrix_UB_33 -0.0114476000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6805 _reflns_number_total 8065 _reflns_odcompleteness_completeness 99.86 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.04 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 1.052 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.113 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 630 _refine_ls_number_reflns 8065 _refine_ls_number_restraints 324 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0271 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+8.9097P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0595 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances F1_1-C2_1 = F3_1-C2_1 1.34 with sigma of 0.02 F2_1-C2_1 1.33 with sigma of 0.02 O1_1-C1_1 1.25 with sigma of 0.02 O2_1-C1_1 1.24 with sigma of 0.02 C1_1-C2_1 1.55 with sigma of 0.02 C1_2-C2_2 1.55 with sigma of 0.02 O2_2-C1_2 1.24 with sigma of 0.02 F1_2-C2_2 = F3_2-C2_2 1.34 with sigma of 0.02 F2_2-C2_2 1.33 with sigma of 0.02 O1_2-C1_2 1.25 with sigma of 0.02 N1_3-C3_3 1.46 with sigma of 0.02 C1_3-O1_3 1.22 with sigma of 0.02 N1_3-C2_3 1.45 with sigma of 0.02 C1_3-N1_3 1.36 with sigma of 0.02 N1_4-C2_4 1.45 with sigma of 0.02 N1_4-C3_4 1.46 with sigma of 0.02 C1_4-O1_4 1.22 with sigma of 0.02 C1_4-N1_4 1.36 with sigma of 0.02 O2_1-C2_1 2.35 with sigma of 0.04 F2_1-C1_1 2.42 with sigma of 0.04 F1_1-F3_1 2.15 with sigma of 0.04 O1_1-O2_1 2.25 with sigma of 0.04 F1_1-F2_1 = F2_1-F3_1 2.16 with sigma of 0.04 F1_1-C1_1 2.37 with sigma of 0.04 F3_1-C1_1 2.39 with sigma of 0.04 O1_1-C2_1 2.38 with sigma of 0.04 F1_2-F3_2 2.15 with sigma of 0.04 O1_2-O2_2 2.25 with sigma of 0.04 F2_2-C1_2 2.42 with sigma of 0.04 F1_2-F2_2 = F2_2-F3_2 2.16 with sigma of 0.04 O2_2-C2_2 2.35 with sigma of 0.04 F1_2-C1_2 2.37 with sigma of 0.04 F3_2-C1_2 2.39 with sigma of 0.04 O1_2-C2_2 2.38 with sigma of 0.04 C1_3-C3_3 2.45 with sigma of 0.04 C1_3-C2_3 2.46 with sigma of 0.04 C1_4-C2_4 2.46 with sigma of 0.04 C1_4-C3_4 2.45 with sigma of 0.04 C1_1-O2_1 \\sim C1_1-O1_1 C1_2-O2_2 \\sim C1_2-O1_2 with sigma of 0.02 C2_1-F1_1 \\sim C2_1-F2_1 \\sim C2_1-F3_1 C2_2-F1_2 \\sim C2_2-F2_2 \\sim C2_2-F3_2 with sigma of 0.02 F1_1-F2_1 \\sim F2_1-F3_1 \\sim F3_1-F1_1 F1_2-F2_2 \\sim F2_2-F3_2 \\sim F3_2-F1_2 with sigma of 0.04 O2_1-C2_1 O2_2-C2_2 with sigma of 0.04 C1_1-F1_1 \\sim C1_1-F2_1 \\sim C1_1-F3_1 C1_2-F1_2 \\sim C1_2-F2_2 \\sim C1_2-F3_2 with sigma of 0.04 C1_1-C2_1 C1_2-C2_2 with sigma of 0.02 O1_1-O2_1 O1_2-O2_2 with sigma of 0.04 C1_3-O1_3 C1_4-O1_4 with sigma of 0.02 C2_3-C3_3 C2_4-C3_4 with sigma of 0.04 N1_3-C1_3 N1_4-C1_4 with sigma of 0.02 C1_3-C2_3 C1_4-C2_4 with sigma of 0.04 N1_3-C2_3 \\sim N1_3-C3_3 N1_4-C2_4 \\sim N1_4-C3_4 with sigma of 0.02 C1_3-C3_3 C1_4-C3_4 with sigma of 0.04 3. Restrained planarity C1_1, C2_1, O1_1, O2_1 C1_2, C2_2, O1_2, O2_2 with sigma of 0.1 C1_3, O1_3, N1_3, C2_3, C3_3 C1_4, O1_4, N1_4, C2_4, C3_4 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1A 5. Rigid body (RIGU) restrains F1_1, F2_1, F3_1, O1_1, O2_1, C1_1, C2_1 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 F1_2, F2_2, F3_2, O1_2, O2_2, C1_2, C2_2 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C1_3, O1_3, N1_3, C2_3, C3_3 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C1_4, O1_4, N1_4, C2_4, C3_4 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Same fragment restrains {O2_2, O1_2, C1_2, C2_2, F2_2, F3_2, F1_2} sigma for 1-2: 0.02, 1-3: 0.02 as in {O2_1, O1_1, C1_1, C2_1, F1_1, F3_1, F2_1} {O1_4, C1_4, N1_4, C3_4, C2_4} sigma for 1-2: 0.02, 1-3: 0.02 as in {O1_3, C1_3, N1_3, C3_3, C2_3} 7. Others Sof(O1B)=Sof(H10C)=Sof(H10D)=Sof(H9BC)=Sof(H9BD)=1-FVAR(1) Sof(O1)=Sof(H10A)=Sof(H10B)=Sof(H9AA)=Sof(H9AB)=FVAR(1) Sof(O2)=Sof(O1)=Sof(C1)=Sof(C2)=Sof(F2)=Sof(F3)=Sof(F1)=1-FVAR(2) Sof(O2)=Sof(O1)=Sof(C1)=Sof(C2)=Sof(F1)=Sof(F3)=Sof(F2)=FVAR(2) Sof(O1)=Sof(C1)=Sof(H1)=Sof(N1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C2)= Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(3) Sof(O1)=Sof(C1)=Sof(H1)=Sof(N1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C2)= Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(3) Sof(O8B)=1-FVAR(4) Sof(O8A)=FVAR(4) 8.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C1(H1A,H1B), C15(H15A,H15B), C14(H14A,H14B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C10(H10C,H10D), C9(H9AA,H9AB), C9(H9BC,H9BD), C8(H8A,H8B), C23(H23A,H23B), C16(H16A,H16B) 8.b Aromatic/amide H refined with riding coordinates: C5(H5), C4(H4), C3(H3), C25(H25), C26(H26), C27(H27), C18(H18), C19(H19), C20(H20), C1(H1), C1(H1) 8.c Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C) ; _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 Bi Bi 0.62819(2) 0.30299(2) 0.64134(2) 0.01666(4) Uani 1 1 d . . . . . O3 O 0.4729(2) 0.3140(2) 0.53168(13) 0.0345(6) Uani 1 1 d . . . . . O2 O 0.5717(3) 0.1187(3) 0.52791(14) 0.0530(9) Uani 1 1 d . . . . . O1 O 0.7310(3) 0.2291(3) 0.51685(16) 0.0272(12) Uani 0.734(9) 1 d . . P A 1 O1B O 0.8033(8) 0.2188(7) 0.4954(6) 0.036(4) Uani 0.266(9) 1 d . . P A 2 O6 O 0.60205(18) 0.31371(18) 0.74192(11) 0.0205(5) Uani 1 1 d . . . . . O7 O 0.6479(2) 0.2639(2) 0.83742(12) 0.0279(6) Uani 1 1 d . . . . . O4 O 0.65921(18) 0.12742(17) 0.65819(11) 0.0211(5) Uani 1 1 d . . . . . O5 O 0.6025(2) -0.03895(19) 0.65470(13) 0.0298(6) Uani 1 1 d . . . . . N3 N 0.8076(2) 0.3843(2) 0.59420(13) 0.0201(6) Uani 1 1 d . . . . . N2 N 0.6580(2) 0.5070(2) 0.65497(13) 0.0199(6) Uani 1 1 d . . . . . N1 N 0.4599(2) 0.4234(2) 0.65077(14) 0.0222(6) Uani 1 1 d . . . . . N5 N 0.7858(2) 0.2852(2) 0.70187(13) 0.0187(6) Uani 1 1 d . . . . . N4 N 0.4732(2) 0.2031(2) 0.66029(13) 0.0202(6) Uani 1 1 d . . . . . C7 C 0.8323(3) 0.4845(3) 0.62632(17) 0.0237(7) Uani 1 1 d . . . . . H7A H 0.879911 0.524443 0.601122 0.028 Uiso 1 1 calc R U . . . H7B H 0.866300 0.468044 0.666528 0.028 Uiso 1 1 calc R U . . . C6 C 0.7434(3) 0.5533(3) 0.63799(16) 0.0223(7) Uani 1 1 d . . . . . C5 C 0.7543(3) 0.6624(3) 0.63644(17) 0.0263(8) Uani 1 1 d . . . . . H5 H 0.814962 0.693466 0.623853 0.032 Uiso 1 1 calc R U . . . C4 C 0.6744(3) 0.7250(3) 0.65371(18) 0.0296(9) Uani 1 1 d . . . . . H4 H 0.680182 0.799643 0.653452 0.036 Uiso 1 1 calc R U . . . C3 C 0.5868(3) 0.6778(3) 0.67122(18) 0.0278(8) Uani 1 1 d . . . . . H3 H 0.531497 0.719396 0.683045 0.033 Uiso 1 1 calc R U . . . C2 C 0.5809(3) 0.5685(3) 0.67124(16) 0.0223(7) Uani 1 1 d . . . . . C1 C 0.4890(3) 0.5122(3) 0.69215(18) 0.0266(8) Uani 1 1 d . . . . . H1A H 0.501429 0.484954 0.734665 0.032 Uiso 1 1 calc R U . . . H1B H 0.432955 0.563044 0.693517 0.032 Uiso 1 1 calc R U . . . C15 C 0.4277(3) 0.4661(3) 0.58957(18) 0.0308(9) Uani 1 1 d . . . . . H15A H 0.484104 0.505330 0.571931 0.037 Uiso 1 1 calc R U . . . H15B H 0.372507 0.516814 0.595416 0.037 Uiso 1 1 calc R U . . . C14 C 0.3932(3) 0.3831(3) 0.54394(19) 0.0335(9) Uani 1 1 d . . . . . H14A H 0.337006 0.342827 0.561113 0.040 Uiso 1 1 calc R U . . . H14B H 0.369242 0.417013 0.504951 0.040 Uiso 1 1 calc R U . . . C13 C 0.4332(4) 0.2191(3) 0.5016(2) 0.0406(10) Uani 1 1 d . . . . . H13A H 0.397005 0.175987 0.531876 0.049 Uiso 1 1 calc R U . . . H13B H 0.385637 0.238780 0.467508 0.049 Uiso 1 1 calc R U . . . C12 C 0.5149(4) 0.1589(4) 0.4772(2) 0.0406(10) Uani 1 1 d . . . . . H12A H 0.488750 0.100420 0.451066 0.049 Uiso 1 1 calc R U . . . H12B H 0.556975 0.204656 0.451514 0.049 Uiso 1 1 calc R U . . . C11 C 0.6597(4) 0.0643(3) 0.5100(2) 0.0462(12) Uani 1 1 d . . . . . H11A H 0.640162 0.005427 0.482041 0.055 Uiso 1 1 calc R U . . . H11B H 0.693152 0.033764 0.547325 0.055 Uiso 1 1 calc R U . . . C10 C 0.7319(4) 0.1337(3) 0.4779(2) 0.0502(13) Uani 1 1 d . . . . . H10A H 0.799335 0.101586 0.477485 0.060 Uiso 0.734(9) 1 calc R U P A 1 H10B H 0.709005 0.149148 0.434807 0.060 Uiso 0.734(9) 1 calc R U P A 1 H10C H 0.774426 0.082479 0.456189 0.060 Uiso 0.266(9) 1 calc R U P A 2 H10D H 0.689895 0.166856 0.444784 0.060 Uiso 0.266(9) 1 calc R U P A 2 C9 C 0.7844(5) 0.3084(4) 0.4886(2) 0.0490(13) Uani 1 1 d . . . . . H9AA H 0.749391 0.327911 0.449203 0.059 Uiso 0.734(9) 1 calc R U P A 1 H9AB H 0.851106 0.280783 0.478360 0.059 Uiso 0.734(9) 1 calc R U P A 1 H9BC H 0.712026 0.308171 0.477729 0.059 Uiso 0.266(9) 1 calc R U P A 2 H9BD H 0.817797 0.326762 0.449740 0.059 Uiso 0.266(9) 1 calc R U P A 2 C8 C 0.7974(3) 0.4034(3) 0.52684(17) 0.0292(8) Uani 1 1 d . . . . . H8A H 0.739330 0.450283 0.518943 0.035 Uiso 1 1 calc R U . . . H8B H 0.857693 0.441234 0.513372 0.035 Uiso 1 1 calc R U . . . C23 C 0.8853(3) 0.3065(3) 0.61082(16) 0.0226(7) Uani 1 1 d . . . . . H23A H 0.952175 0.336721 0.603712 0.027 Uiso 1 1 calc R U . . . H23B H 0.876913 0.242957 0.584557 0.027 Uiso 1 1 calc R U . . . C24 C 0.8769(3) 0.2770(2) 0.67813(17) 0.0200(7) Uani 1 1 d . . . . . C25 C 0.9583(3) 0.2448(3) 0.71499(18) 0.0251(8) Uani 1 1 d . . . . . H25 H 1.022662 0.238832 0.697966 0.030 Uiso 1 1 calc R U . . . C26 C 0.9443(3) 0.2218(3) 0.7765(2) 0.0323(9) Uani 1 1 d . . . . . H26 H 0.998962 0.198501 0.802127 0.039 Uiso 1 1 calc R U . . . C27 C 0.8499(3) 0.2327(3) 0.80106(18) 0.0278(8) Uani 1 1 d . . . . . H27 H 0.838960 0.218801 0.843569 0.033 Uiso 1 1 calc R U . . . C28 C 0.7726(3) 0.2643(3) 0.76156(16) 0.0203(7) Uani 1 1 d . . . . . C29 C 0.6673(3) 0.2803(2) 0.78332(17) 0.0214(7) Uani 1 1 d . . . . . C16 C 0.3785(3) 0.3630(3) 0.67956(19) 0.0277(8) Uani 1 1 d . . . . . H16A H 0.313481 0.390205 0.663387 0.033 Uiso 1 1 calc R U . . . H16B H 0.381626 0.375496 0.724845 0.033 Uiso 1 1 calc R U . . . C17 C 0.3826(3) 0.2455(3) 0.66792(17) 0.0251(8) Uani 1 1 d . . . . . C18 C 0.2988(3) 0.1830(3) 0.67003(19) 0.0331(9) Uani 1 1 d . . . . . H18 H 0.234932 0.214238 0.674684 0.040 Uiso 1 1 calc R U . . . C19 C 0.3077(3) 0.0746(3) 0.6654(2) 0.0347(9) Uani 1 1 d . . . . . H19 H 0.250200 0.030803 0.666705 0.042 Uiso 1 1 calc R U . . . C20 C 0.4015(3) 0.0306(3) 0.65871(17) 0.0280(8) Uani 1 1 d . . . . . H20 H 0.409610 -0.043560 0.655360 0.034 Uiso 1 1 calc R U . . . C21 C 0.4836(3) 0.0977(3) 0.65705(15) 0.0213(7) Uani 1 1 d . . . . . C22 C 0.5891(3) 0.0566(3) 0.65563(16) 0.0206(7) Uani 1 1 d . . . . . O8A O -0.0823(4) 0.4567(4) 0.3937(2) 0.049(2) Uani 0.772(13) 1 d . . P B 1 O8B O -0.1366(12) 0.534(2) 0.3847(7) 0.078(9) Uani 0.228(13) 1 d . . P B 2 O2_1 O 0.1466(4) 0.3399(5) 0.5777(4) 0.084(3) Uani 0.655(8) 1 d D . P C 1 O1_1 O 0.0621(6) 0.3534(6) 0.4830(4) 0.090(3) Uani 0.655(8) 1 d D U P C 1 C1_1 C 0.1063(5) 0.3071(6) 0.5289(4) 0.054(2) Uani 0.655(8) 1 d D U P C 1 C2_1 C 0.1092(7) 0.1847(5) 0.5245(4) 0.0411(19) Uani 0.655(8) 1 d D U P C 1 F1_1 F 0.1168(9) 0.1363(7) 0.5784(4) 0.147(5) Uani 0.655(8) 1 d D U P C 1 F3_1 F 0.1856(9) 0.1532(10) 0.4926(6) 0.102(4) Uani 0.655(8) 1 d D U P C 1 F2_1 F 0.0285(8) 0.1459(7) 0.4983(6) 0.075(3) Uani 0.655(8) 1 d D U P C 1 O2_2 O 0.1158(12) 0.3603(10) 0.5139(7) 0.083(5) Uani 0.345(8) 1 d D U P C 2 O1_2 O 0.0167(10) 0.2988(9) 0.4309(5) 0.086(4) Uani 0.345(8) 1 d D . P C 2 C1_2 C 0.0682(10) 0.2912(9) 0.4822(6) 0.065(4) Uani 0.345(8) 1 d D U P C 2 C2_2 C 0.0912(13) 0.1824(9) 0.5120(7) 0.068(5) Uani 0.345(8) 1 d D U P C 2 F2_2 F 0.1757(17) 0.142(2) 0.4929(11) 0.112(9) Uani 0.345(8) 1 d D U P C 2 F3_2 F 0.1027(11) 0.1803(14) 0.5739(6) 0.122(7) Uani 0.345(8) 1 d D U P C 2 F1_2 F 0.0213(17) 0.1135(11) 0.4995(10) 0.073(5) Uani 0.345(8) 1 d D U P C 2 O1_3 O -0.0953(6) 0.5118(12) 0.7742(6) 0.044(3) Uani 0.742(8) 1 d D U P D 1 C1_3 C -0.0102(4) 0.4920(4) 0.7580(2) 0.0271(13) Uani 0.742(8) 1 d D . P D 1 H1_3 H 0.000804 0.492991 0.714776 0.032 Uiso 0.742(8) 1 calc R U P D 1 N1_3 N 0.0687(5) 0.4693(8) 0.7951(3) 0.0404(18) Uani 0.742(8) 1 d D U P D 1 C3_3 C 0.0592(9) 0.4616(8) 0.8611(3) 0.093(4) Uani 0.742(8) 1 d D U P D 1 H3A_3 H -0.005340 0.490862 0.872741 0.140 Uiso 0.742(8) 1 calc R U P D 1 H3B_3 H 0.113329 0.501263 0.881889 0.140 Uiso 0.742(8) 1 calc R U P D 1 H3C_3 H 0.063135 0.387396 0.873635 0.140 Uiso 0.742(8) 1 calc R U P D 1 C2_3 C 0.1648(5) 0.4468(8) 0.7686(4) 0.066(3) Uani 0.742(8) 1 d D U P D 1 H2A_3 H 0.183886 0.373720 0.777806 0.099 Uiso 0.742(8) 1 calc R U P D 1 H2B_3 H 0.215430 0.494678 0.786436 0.099 Uiso 0.742(8) 1 calc R U P D 1 H2C_3 H 0.160104 0.456824 0.723552 0.099 Uiso 0.742(8) 1 calc R U P D 1 O1_4 O -0.0897(19) 0.490(3) 0.7745(17) 0.037(7) Uani 0.258(8) 1 d D U P D 2 C1_4 C -0.0309(9) 0.4888(12) 0.8194(7) 0.033(4) Uani 0.258(8) 1 d D . P D 2 H1_4 H -0.058159 0.500079 0.858952 0.040 Uiso 0.258(8) 1 calc R U P D 2 N1_4 N 0.0679(10) 0.4730(19) 0.8178(7) 0.031(4) Uani 0.258(8) 1 d D U P D 2 C3_4 C 0.1166(14) 0.4560(17) 0.7594(7) 0.042(5) Uani 0.258(8) 1 d D U P D 2 H3A_4 H 0.066591 0.457895 0.725300 0.063 Uiso 0.258(8) 1 calc R U P D 2 H3B_4 H 0.149802 0.387126 0.760130 0.063 Uiso 0.258(8) 1 calc R U P D 2 H3C_4 H 0.166287 0.511531 0.753322 0.063 Uiso 0.258(8) 1 calc R U P D 2 C2_4 C 0.1301(13) 0.4747(16) 0.8737(7) 0.048(5) Uani 0.258(8) 1 d D U P D 2 H2A_4 H 0.090314 0.497612 0.908610 0.073 Uiso 0.258(8) 1 calc R U P D 2 H2B_4 H 0.185779 0.523746 0.868452 0.073 Uiso 0.258(8) 1 calc R U P D 2 H2C_4 H 0.156429 0.403769 0.881960 0.073 Uiso 0.258(8) 1 calc R U P D 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 Bi 0.01657(6) 0.01272(6) 0.02097(7) 0.00179(5) 0.00509(4) 0.00175(5) O3 0.0373(16) 0.0356(15) 0.0302(15) -0.0021(12) -0.0045(12) 0.0123(13) O2 0.079(3) 0.054(2) 0.0250(15) -0.0070(14) -0.0052(16) 0.0327(18) O1 0.030(3) 0.0247(19) 0.027(2) -0.0030(14) 0.0064(16) -0.0029(15) O1B 0.022(7) 0.016(6) 0.069(9) -0.013(5) -0.011(6) 0.010(4) O6 0.0201(12) 0.0195(11) 0.0219(12) -0.0006(10) 0.0037(9) 0.0017(10) O7 0.0285(15) 0.0318(14) 0.0237(14) 0.0059(11) 0.0056(11) 0.0025(11) O4 0.0239(13) 0.0108(10) 0.0289(13) 0.0032(9) 0.0042(10) 0.0022(9) O5 0.0323(15) 0.0146(12) 0.0427(17) 0.0006(11) 0.0013(12) -0.0001(10) N3 0.0222(15) 0.0149(13) 0.0237(15) 0.0010(11) 0.0078(12) 0.0015(11) N2 0.0262(16) 0.0109(13) 0.0230(15) -0.0013(11) 0.0055(12) 0.0012(11) N1 0.0218(15) 0.0182(14) 0.0269(16) -0.0005(12) 0.0052(12) 0.0023(12) N5 0.0186(14) 0.0126(13) 0.0251(15) 0.0008(11) 0.0020(11) 0.0013(11) N4 0.0198(14) 0.0205(14) 0.0204(14) 0.0008(12) 0.0034(11) -0.0016(12) C7 0.0270(19) 0.0145(16) 0.0300(19) 0.0011(14) 0.0059(15) -0.0023(14) C6 0.029(2) 0.0145(15) 0.0237(18) 0.0011(13) 0.0034(15) -0.0001(14) C5 0.031(2) 0.0187(16) 0.029(2) 0.0008(14) 0.0019(16) -0.0049(15) C4 0.046(2) 0.0099(15) 0.033(2) -0.0020(14) 0.0023(18) 0.0000(15) C3 0.035(2) 0.0186(18) 0.030(2) -0.0033(14) 0.0050(16) 0.0078(15) C2 0.0265(19) 0.0195(17) 0.0210(17) -0.0014(13) 0.0026(14) 0.0051(14) C1 0.030(2) 0.0184(17) 0.032(2) -0.0029(14) 0.0089(16) 0.0059(15) C15 0.031(2) 0.0269(19) 0.035(2) 0.0042(16) 0.0007(17) 0.0101(16) C14 0.030(2) 0.038(2) 0.032(2) 0.0035(17) -0.0053(17) 0.0048(17) C13 0.044(3) 0.042(2) 0.036(2) -0.0032(19) -0.005(2) -0.004(2) C12 0.051(3) 0.040(2) 0.030(2) -0.0061(18) -0.009(2) -0.001(2) C11 0.076(4) 0.031(2) 0.031(2) -0.0090(18) -0.004(2) 0.020(2) C10 0.069(4) 0.026(2) 0.054(3) -0.004(2) -0.021(3) -0.001(2) C9 0.087(4) 0.034(2) 0.026(2) 0.0019(18) 0.008(2) -0.018(3) C8 0.038(2) 0.0223(18) 0.0281(19) 0.0054(15) 0.0065(16) 0.0010(16) C23 0.0208(17) 0.0173(16) 0.0299(18) 0.0017(14) 0.0079(14) 0.0006(14) C24 0.0190(17) 0.0122(15) 0.0289(18) -0.0011(13) 0.0044(14) -0.0018(12) C25 0.0177(18) 0.0212(17) 0.037(2) 0.0013(15) 0.0045(15) 0.0031(14) C26 0.023(2) 0.031(2) 0.043(2) 0.0046(17) -0.0043(17) 0.0042(15) C27 0.029(2) 0.0261(18) 0.029(2) 0.0040(15) 0.0027(16) 0.0009(15) C28 0.0210(18) 0.0132(14) 0.0270(18) 0.0016(13) 0.0045(14) 0.0014(13) C29 0.0230(18) 0.0125(15) 0.0290(19) 0.0000(13) 0.0053(15) -0.0016(13) C16 0.0204(19) 0.0265(19) 0.037(2) -0.0016(16) 0.0104(16) 0.0054(15) C17 0.0200(18) 0.0285(19) 0.0272(19) -0.0022(15) 0.0056(15) -0.0003(15) C18 0.0194(19) 0.040(2) 0.041(2) -0.0043(18) 0.0073(16) -0.0033(17) C19 0.027(2) 0.035(2) 0.042(2) -0.0044(18) 0.0079(18) -0.0143(17) C20 0.032(2) 0.0243(18) 0.028(2) -0.0014(15) 0.0043(16) -0.0069(16) C21 0.0245(18) 0.0206(16) 0.0191(16) 0.0026(13) 0.0037(14) -0.0016(14) C22 0.0292(19) 0.0146(15) 0.0180(17) 0.0024(12) -0.0012(14) -0.0006(14) O8A 0.053(4) 0.055(3) 0.041(3) -0.014(2) 0.017(2) -0.024(3) O8B 0.026(9) 0.17(3) 0.041(9) 0.038(11) 0.010(7) -0.003(12) O2_1 0.027(3) 0.074(4) 0.152(7) -0.053(5) 0.001(3) 0.006(3) O1_1 0.063(5) 0.073(6) 0.134(8) 0.063(6) 0.028(4) -0.003(4) C1_1 0.033(4) 0.040(4) 0.092(6) -0.009(4) 0.036(3) -0.008(3) C2_1 0.043(4) 0.038(4) 0.043(5) -0.008(3) 0.009(3) -0.003(3) F1_1 0.258(13) 0.093(6) 0.086(5) 0.035(4) -0.066(6) -0.095(7) F3_1 0.039(4) 0.077(6) 0.191(11) -0.030(7) 0.029(6) 0.025(4) F2_1 0.044(4) 0.048(5) 0.132(7) -0.035(5) -0.007(4) 0.002(3) O2_2 0.101(13) 0.046(7) 0.102(12) -0.011(8) 0.002(9) -0.032(8) O1_2 0.118(10) 0.085(8) 0.057(6) -0.030(6) 0.052(6) -0.070(7) C1_2 0.082(10) 0.045(7) 0.072(8) -0.027(6) 0.055(6) -0.029(7) C2_2 0.074(12) 0.052(7) 0.079(10) -0.033(7) 0.018(8) -0.005(7) F2_2 0.072(11) 0.094(14) 0.17(2) -0.068(14) 0.028(12) 0.002(8) F3_2 0.089(10) 0.195(17) 0.080(9) -0.025(8) -0.023(7) 0.108(11) F1_2 0.083(9) 0.043(8) 0.095(10) 0.017(7) 0.021(7) -0.010(7) O1_3 0.031(3) 0.045(6) 0.055(4) -0.005(3) 0.014(3) 0.005(3) C1_3 0.025(3) 0.024(3) 0.032(3) -0.002(2) 0.001(2) -0.002(2) N1_3 0.042(3) 0.034(3) 0.044(4) -0.004(4) -0.016(3) 0.003(3) C3_3 0.155(11) 0.086(7) 0.036(4) -0.011(4) -0.038(5) 0.022(7) C2_3 0.030(4) 0.050(4) 0.117(7) -0.014(4) -0.021(4) 0.006(4) O1_4 0.035(10) 0.037(14) 0.039(9) -0.006(8) 0.000(7) 0.006(7) C1_4 0.035(6) 0.033(8) 0.031(7) -0.007(6) 0.004(5) -0.006(6) N1_4 0.031(6) 0.028(8) 0.033(9) 0.005(9) 0.005(5) -0.010(6) C3_4 0.043(12) 0.042(11) 0.042(9) 0.008(8) 0.014(9) -0.005(11) C2_4 0.052(11) 0.050(11) 0.043(9) 0.008(8) -0.010(8) -0.007(10) _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 Bi O6 2.214(2) . ? Bi O4 2.292(2) . ? Bi N2 2.633(3) . ? Bi N1 2.734(3) . ? Bi N5 2.459(3) . ? Bi N4 2.476(3) . ? O3 C14 1.412(5) . ? O3 C13 1.461(5) . ? O2 C12 1.409(5) . ? O2 C11 1.428(6) . ? O1 C10 1.474(6) . ? O1 C9 1.386(6) . ? O1B C10 1.484(11) . ? O1B C9 1.172(10) . ? O6 C29 1.301(4) . ? O7 C29 1.222(4) . ? O4 C22 1.299(4) . ? O5 C22 1.225(4) . ? N3 C7 1.480(4) . ? N3 C8 1.476(5) . ? N3 C23 1.470(4) . ? N2 C6 1.346(5) . ? N2 C2 1.348(4) . ? N1 C1 1.483(5) . ? N1 C15 1.480(5) . ? N1 C16 1.483(5) . ? N5 C24 1.340(4) . ? N5 C28 1.332(4) . ? N4 C17 1.341(5) . ? N4 C21 1.346(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C6 1.504(5) . ? C6 C5 1.391(5) . ? C5 H5 0.9500 . ? C5 C4 1.391(6) . ? C4 H4 0.9500 . ? C4 C3 1.379(6) . ? C3 H3 0.9500 . ? C3 C2 1.389(5) . ? C2 C1 1.504(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C14 1.505(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C12 1.445(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C10 1.493(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 H10C 0.9900 . ? C10 H10D 0.9900 . ? C9 H9AA 0.9900 . ? C9 H9AB 0.9900 . ? C9 H9BC 0.9900 . ? C9 H9BD 0.9900 . ? C9 C8 1.468(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.508(5) . ? C24 C25 1.391(5) . ? C25 H25 0.9500 . ? C25 C26 1.379(6) . ? C26 H26 0.9500 . ? C26 C27 1.392(6) . ? C27 H27 0.9500 . ? C27 C28 1.381(5) . ? C28 C29 1.512(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.513(5) . ? C17 C18 1.375(5) . ? C18 H18 0.9500 . ? C18 C19 1.385(6) . ? C19 H19 0.9500 . ? C19 C20 1.385(6) . ? C20 H20 0.9500 . ? C20 C21 1.390(5) . ? C21 C22 1.507(5) . ? O2_1 C1_1 1.241(8) . ? O1_1 C1_1 1.281(8) . ? C1_1 C2_1 1.556(9) . ? C2_1 F1_1 1.316(8) . ? C2_1 F3_1 1.312(8) . ? C2_1 F2_1 1.301(8) . ? O2_2 C1_2 1.271(10) . ? O1_2 C1_2 1.290(10) . ? C1_2 C2_2 1.549(11) . ? C2_2 F2_2 1.319(11) . ? C2_2 F3_2 1.341(11) . ? C2_2 F1_2 1.303(10) . ? O1_3 C1_3 1.228(11) . ? C1_3 H1_3 0.9500 . ? C1_3 N1_3 1.336(7) . ? N1_3 C3_3 1.438(8) . ? N1_3 C2_3 1.453(8) . ? C3_3 H3A_3 0.9800 . ? C3_3 H3B_3 0.9800 . ? C3_3 H3C_3 0.9800 . ? C2_3 H2A_3 0.9800 . ? C2_3 H2B_3 0.9800 . ? C2_3 H2C_3 0.9800 . ? O1_4 C1_4 1.229(16) . ? C1_4 H1_4 0.9500 . ? C1_4 N1_4 1.339(11) . ? N1_4 C3_4 1.452(11) . ? N1_4 C2_4 1.446(11) . ? C3_4 H3A_4 0.9800 . ? C3_4 H3B_4 0.9800 . ? C3_4 H3C_4 0.9800 . ? C2_4 H2A_4 0.9800 . ? C2_4 H2B_4 0.9800 . ? C2_4 H2C_4 0.9800 . ? 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 O6 Bi O4 86.40(8) . . ? O6 Bi N2 81.83(8) . . ? O6 Bi N1 74.80(9) . . ? O6 Bi N5 69.08(9) . . ? O6 Bi N4 73.23(9) . . ? O4 Bi N2 155.61(9) . . ? O4 Bi N1 132.55(9) . . ? O4 Bi N5 71.22(9) . . ? O4 Bi N4 67.99(9) . . ? N2 Bi N1 64.25(9) . . ? N5 Bi N2 84.61(9) . . ? N5 Bi N1 135.05(9) . . ? N5 Bi N4 125.13(9) . . ? N4 Bi N2 127.54(9) . . ? N4 Bi N1 64.96(9) . . ? C14 O3 C13 109.1(3) . . ? C12 O2 C11 113.2(3) . . ? C9 O1 C10 109.3(4) . . ? C9 O1B C10 122.5(9) . . ? C29 O6 Bi 122.1(2) . . ? C22 O4 Bi 122.5(2) . . ? C8 N3 C7 109.5(3) . . ? C23 N3 C7 108.4(3) . . ? C23 N3 C8 113.2(3) . . ? C6 N2 Bi 121.7(2) . . ? C6 N2 C2 118.8(3) . . ? C2 N2 Bi 118.9(2) . . ? C1 N1 Bi 105.5(2) . . ? C1 N1 C16 108.8(3) . . ? C15 N1 Bi 110.9(2) . . ? C15 N1 C1 108.9(3) . . ? C15 N1 C16 111.4(3) . . ? C16 N1 Bi 111.1(2) . . ? C24 N5 Bi 125.4(2) . . ? C28 N5 Bi 113.3(2) . . ? C28 N5 C24 120.2(3) . . ? C17 N4 Bi 125.5(2) . . ? C17 N4 C21 120.0(3) . . ? C21 N4 Bi 114.3(2) . . ? N3 C7 H7A 108.7 . . ? N3 C7 H7B 108.7 . . ? N3 C7 C6 114.2(3) . . ? H7A C7 H7B 107.6 . . ? C6 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? N2 C6 C7 118.4(3) . . ? N2 C6 C5 122.1(3) . . ? C5 C6 C7 119.3(3) . . ? C6 C5 H5 120.7 . . ? C6 C5 C4 118.6(4) . . ? C4 C5 H5 120.7 . . ? C5 C4 H4 120.2 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C4 C3 H3 120.6 . . ? C4 C3 C2 118.8(3) . . ? C2 C3 H3 120.6 . . ? N2 C2 C3 122.2(3) . . ? N2 C2 C1 116.3(3) . . ? C3 C2 C1 121.4(3) . . ? N1 C1 C2 112.5(3) . . ? N1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N1 C15 H15A 108.8 . . ? N1 C15 H15B 108.8 . . ? N1 C15 C14 113.8(3) . . ? H15A C15 H15B 107.7 . . ? C14 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? O3 C14 C15 109.8(3) . . ? O3 C14 H14A 109.7 . . ? O3 C14 H14B 109.7 . . ? C15 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? O3 C13 H13A 109.9 . . ? O3 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C12 C13 O3 109.1(4) . . ? C12 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? O2 C12 C13 107.8(4) . . ? O2 C12 H12A 110.2 . . ? O2 C12 H12B 110.2 . . ? C13 C12 H12A 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? O2 C11 H11A 109.0 . . ? O2 C11 H11B 109.0 . . ? O2 C11 C10 113.1(4) . . ? H11A C11 H11B 107.8 . . ? C10 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? O1 C10 C11 101.6(4) . . ? O1 C10 H10A 111.4 . . ? O1 C10 H10B 111.4 . . ? O1B C10 C11 137.0(7) . . ? O1B C10 H10C 102.9 . . ? O1B C10 H10D 102.9 . . ? C11 C10 H10A 111.4 . . ? C11 C10 H10B 111.4 . . ? C11 C10 H10C 102.9 . . ? C11 C10 H10D 102.9 . . ? H10A C10 H10B 109.3 . . ? H10C C10 H10D 105.1 . . ? O1 C9 H9AA 108.8 . . ? O1 C9 H9AB 108.8 . . ? O1 C9 C8 113.7(4) . . ? O1B C9 H9BC 103.5 . . ? O1B C9 H9BD 103.5 . . ? O1B C9 C8 134.6(7) . . ? H9AA C9 H9AB 107.7 . . ? H9BC C9 H9BD 105.3 . . ? C8 C9 H9AA 108.8 . . ? C8 C9 H9AB 108.8 . . ? C8 C9 H9BC 103.5 . . ? C8 C9 H9BD 103.5 . . ? N3 C8 H8A 108.5 . . ? N3 C8 H8B 108.5 . . ? C9 C8 N3 115.2(3) . . ? C9 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? N3 C23 H23A 109.8 . . ? N3 C23 H23B 109.8 . . ? N3 C23 C24 109.2(3) . . ? H23A C23 H23B 108.3 . . ? C24 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? N5 C24 C23 116.4(3) . . ? N5 C24 C25 120.6(3) . . ? C25 C24 C23 123.0(3) . . ? C24 C25 H25 120.4 . . ? C26 C25 C24 119.1(3) . . ? C26 C25 H25 120.4 . . ? C25 C26 H26 120.1 . . ? C25 C26 C27 119.7(4) . . ? C27 C26 H26 120.1 . . ? C26 C27 H27 121.1 . . ? C28 C27 C26 117.8(4) . . ? C28 C27 H27 121.1 . . ? N5 C28 C27 122.4(3) . . ? N5 C28 C29 115.2(3) . . ? C27 C28 C29 122.4(3) . . ? O6 C29 C28 116.3(3) . . ? O7 C29 O6 123.6(3) . . ? O7 C29 C28 120.1(3) . . ? N1 C16 H16A 108.7 . . ? N1 C16 H16B 108.7 . . ? N1 C16 C17 114.1(3) . . ? H16A C16 H16B 107.6 . . ? C17 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? N4 C17 C16 116.9(3) . . ? N4 C17 C18 121.0(4) . . ? C18 C17 C16 121.8(3) . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.8(4) . . ? C19 C18 H18 120.1 . . ? C18 C19 H19 120.4 . . ? C18 C19 C20 119.2(4) . . ? C20 C19 H19 120.4 . . ? C19 C20 H20 120.8 . . ? C19 C20 C21 118.4(3) . . ? C21 C20 H20 120.8 . . ? N4 C21 C20 121.6(3) . . ? N4 C21 C22 116.2(3) . . ? C20 C21 C22 122.1(3) . . ? O4 C22 C21 115.9(3) . . ? O5 C22 O4 125.3(3) . . ? O5 C22 C21 118.7(3) . . ? O2_1 C1_1 O1_1 133.0(8) . . ? O2_1 C1_1 C2_1 111.9(7) . . ? O1_1 C1_1 C2_1 115.0(7) . . ? F1_1 C2_1 C1_1 114.5(7) . . ? F3_1 C2_1 C1_1 111.0(7) . . ? F3_1 C2_1 F1_1 106.3(8) . . ? F2_1 C2_1 C1_1 112.4(7) . . ? F2_1 C2_1 F1_1 104.4(7) . . ? F2_1 C2_1 F3_1 107.9(8) . . ? O2_2 C1_2 O1_2 131.0(11) . . ? O2_2 C1_2 C2_2 107.5(10) . . ? O1_2 C1_2 C2_2 121.1(9) . . ? F2_2 C2_2 C1_2 112.3(12) . . ? F2_2 C2_2 F3_2 103.3(11) . . ? F3_2 C2_2 C1_2 116.6(11) . . ? F1_2 C2_2 C1_2 112.3(10) . . ? F1_2 C2_2 F2_2 107.0(12) . . ? F1_2 C2_2 F3_2 104.6(12) . . ? O1_3 C1_3 H1_3 116.6 . . ? O1_3 C1_3 N1_3 126.7(8) . . ? N1_3 C1_3 H1_3 116.6 . . ? C1_3 N1_3 C3_3 121.1(7) . . ? C1_3 N1_3 C2_3 120.0(6) . . ? C3_3 N1_3 C2_3 118.9(7) . . ? N1_3 C3_3 H3A_3 109.5 . . ? N1_3 C3_3 H3B_3 109.5 . . ? N1_3 C3_3 H3C_3 109.5 . . ? H3A_3 C3_3 H3B_3 109.5 . . ? H3A_3 C3_3 H3C_3 109.5 . . ? H3B_3 C3_3 H3C_3 109.5 . . ? N1_3 C2_3 H2A_3 109.5 . . ? N1_3 C2_3 H2B_3 109.5 . . ? N1_3 C2_3 H2C_3 109.5 . . ? H2A_3 C2_3 H2B_3 109.5 . . ? H2A_3 C2_3 H2C_3 109.5 . . ? H2B_3 C2_3 H2C_3 109.5 . . ? O1_4 C1_4 H1_4 116.9 . . ? O1_4 C1_4 N1_4 126.2(19) . . ? N1_4 C1_4 H1_4 116.9 . . ? C1_4 N1_4 C3_4 120.9(11) . . ? C1_4 N1_4 C2_4 121.4(11) . . ? C2_4 N1_4 C3_4 117.7(11) . . ? N1_4 C3_4 H3A_4 109.5 . . ? N1_4 C3_4 H3B_4 109.5 . . ? N1_4 C3_4 H3C_4 109.5 . . ? H3A_4 C3_4 H3B_4 109.5 . . ? H3A_4 C3_4 H3C_4 109.5 . . ? H3B_4 C3_4 H3C_4 109.5 . . ? N1_4 C2_4 H2A_4 109.5 . . ? N1_4 C2_4 H2B_4 109.5 . . ? N1_4 C2_4 H2C_4 109.5 . . ? H2A_4 C2_4 H2B_4 109.5 . . ? H2A_4 C2_4 H2C_4 109.5 . . ? H2B_4 C2_4 H2C_4 109.5 . . ? 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 Bi O6 C29 O7 -163.7(3) . . . . ? Bi O6 C29 C28 17.6(4) . . . . ? Bi O4 C22 O5 168.1(3) . . . . ? Bi O4 C22 C21 -14.9(4) . . . . ? Bi N2 C6 C7 -15.5(4) . . . . ? Bi N2 C6 C5 170.4(3) . . . . ? Bi N2 C2 C3 -171.1(3) . . . . ? Bi N2 C2 C1 11.4(4) . . . . ? Bi N1 C1 C2 52.4(3) . . . . ? Bi N1 C15 C14 66.2(4) . . . . ? Bi N1 C16 C17 -29.2(4) . . . . ? Bi N5 C24 C23 15.1(4) . . . . ? Bi N5 C24 C25 -166.1(2) . . . . ? Bi N5 C28 C27 168.0(3) . . . . ? Bi N5 C28 C29 -13.4(3) . . . . ? Bi N4 C17 C16 -13.8(5) . . . . ? Bi N4 C17 C18 171.3(3) . . . . ? Bi N4 C21 C20 -171.7(3) . . . . ? Bi N4 C21 C22 12.0(4) . . . . ? O3 C13 C12 O2 68.7(5) . . . . ? O2 C11 C10 O1 43.7(5) . . . . ? O2 C11 C10 O1B 73.5(9) . . . . ? O1 C9 C8 N3 33.6(6) . . . . ? O1B C9 C8 N3 -22.4(12) . . . . ? N3 C7 C6 N2 39.2(5) . . . . ? N3 C7 C6 C5 -146.5(3) . . . . ? N3 C23 C24 N5 27.6(4) . . . . ? N3 C23 C24 C25 -151.2(3) . . . . ? N2 C6 C5 C4 0.7(6) . . . . ? N2 C2 C1 N1 -45.9(4) . . . . ? N1 C15 C14 O3 -62.5(4) . . . . ? N1 C16 C17 N4 29.6(5) . . . . ? N1 C16 C17 C18 -155.6(4) . . . . ? N5 C24 C25 C26 -0.3(5) . . . . ? N5 C28 C29 O6 -0.8(4) . . . . ? N5 C28 C29 O7 -179.5(3) . . . . ? N4 C17 C18 C19 1.2(6) . . . . ? N4 C21 C22 O4 0.5(4) . . . . ? N4 C21 C22 O5 177.7(3) . . . . ? C7 N3 C8 C9 173.2(4) . . . . ? C7 N3 C23 C24 69.1(3) . . . . ? C7 C6 C5 C4 -173.3(3) . . . . ? C6 N2 C2 C3 -0.2(5) . . . . ? C6 N2 C2 C1 -177.7(3) . . . . ? C6 C5 C4 C3 -0.6(6) . . . . ? C5 C4 C3 C2 0.2(6) . . . . ? C4 C3 C2 N2 0.3(6) . . . . ? C4 C3 C2 C1 177.6(4) . . . . ? C3 C2 C1 N1 136.6(4) . . . . ? C2 N2 C6 C7 173.8(3) . . . . ? C2 N2 C6 C5 -0.3(5) . . . . ? C1 N1 C15 C14 -178.2(3) . . . . ? C1 N1 C16 C17 -144.9(3) . . . . ? C15 N1 C1 C2 -66.6(4) . . . . ? C15 N1 C16 C17 95.0(4) . . . . ? C14 O3 C13 C12 167.9(3) . . . . ? C13 O3 C14 C15 164.7(3) . . . . ? C12 O2 C11 C10 62.8(5) . . . . ? C11 O2 C12 C13 -175.3(4) . . . . ? C10 O1 C9 C8 -173.7(4) . . . . ? C10 O1B C9 C8 135.5(9) . . . . ? C9 O1 C10 C11 -171.8(4) . . . . ? C9 O1B C10 C11 -99.5(13) . . . . ? C8 N3 C7 C6 82.2(4) . . . . ? C8 N3 C23 C24 -169.3(3) . . . . ? C23 N3 C7 C6 -153.9(3) . . . . ? C23 N3 C8 C9 52.2(5) . . . . ? C23 C24 C25 C26 178.4(3) . . . . ? C24 N5 C28 C27 -0.8(5) . . . . ? C24 N5 C28 C29 177.8(3) . . . . ? C24 C25 C26 C27 -1.1(6) . . . . ? C25 C26 C27 C28 1.5(6) . . . . ? C26 C27 C28 N5 -0.6(5) . . . . ? C26 C27 C28 C29 -179.1(3) . . . . ? C27 C28 C29 O6 177.8(3) . . . . ? C27 C28 C29 O7 -0.9(5) . . . . ? C28 N5 C24 C23 -177.6(3) . . . . ? C28 N5 C24 C25 1.2(5) . . . . ? C16 N1 C1 C2 171.7(3) . . . . ? C16 N1 C15 C14 -58.2(4) . . . . ? C16 C17 C18 C19 -173.4(4) . . . . ? C17 N4 C21 C20 2.9(5) . . . . ? C17 N4 C21 C22 -173.4(3) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 0.1(6) . . . . ? C19 C20 C21 N4 -1.6(5) . . . . ? C19 C20 C21 C22 174.5(3) . . . . ? C20 C21 C22 O4 -175.7(3) . . . . ? C20 C21 C22 O5 1.5(5) . . . . ? C21 N4 C17 C16 172.2(3) . . . . ? C21 N4 C17 C18 -2.7(5) . . . . ? O2_1 C1_1 C2_1 F1_1 24.4(10) . . . . ? O2_1 C1_1 C2_1 F3_1 -95.8(10) . . . . ? O2_1 C1_1 C2_1 F2_1 143.3(9) . . . . ? O1_1 C1_1 C2_1 F1_1 -154.4(9) . . . . ? O1_1 C1_1 C2_1 F3_1 85.3(10) . . . . ? O1_1 C1_1 C2_1 F2_1 -35.5(10) . . . . ? O2_2 C1_2 C2_2 F2_2 -83.7(17) . . . . ? O2_2 C1_2 C2_2 F3_2 35.2(17) . . . . ? O2_2 C1_2 C2_2 F1_2 155.8(16) . . . . ? O1_2 C1_2 C2_2 F2_2 90.5(16) . . . . ? O1_2 C1_2 C2_2 F3_2 -150.7(14) . . . . ? O1_2 C1_2 C2_2 F1_2 -30.1(18) . . . . ? O1_3 C1_3 N1_3 C3_3 2.5(15) . . . . ? O1_3 C1_3 N1_3 C2_3 179.5(11) . . . . ? O1_4 C1_4 N1_4 C3_4 1(3) . . . . ? O1_4 C1_4 N1_4 C2_4 179(3) . . . . ? _shelx_res_file ; TITL rah20_abs_a.res in P2(1)/c rah20_abs.res created by SHELXL-2016/6 at 14:36:10 on 04-Dec-2020 REM Old TITL Rah20_abs in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.101, Rweak 0.004, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C41 B N7 O8 F Bi CELL 0.71073 13.3865 12.6811 21.5862 90 91.723 90 ZERR 4 0.0003 0.0002 0.0004 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Bi F N O UNIT 136 160 4 12 24 44 DFIX_1 1.34 F1 C2 F3 C2 DANG_1 2.35 O2 C2 DFIX_1 1.33 F2 C2 DANG_1 2.42 F2 C1 DFIX_1 1.25 O1 C1 RIGU_1 F1 F2 F3 O1 O2 C1 C2 DFIX_1 1.24 O2 C1 DANG_1 2.15 F1 F3 DFIX_1 1.55 C1 C2 DANG_1 2.25 O1 O2 DANG_1 2.16 F1 F2 F2 F3 DANG_1 2.37 F1 C1 DANG_1 2.39 F3 C1 DANG_1 2.38 O1 C2 SADI_TFA C1 O2 C1 O1 SADI_TFA C2 F1 C2 F2 C2 F3 DANG_2 2.15 F1 F3 SADI_TFA 0.04 F1 F2 F2 F3 F3 F1 DANG_2 2.25 O1 O2 DANG_2 2.42 F2 C1 SADI_TFA 0.04 O2 C2 RIGU_2 F1 F2 F3 O1 O2 C1 C2 SADI_TFA 0.04 C1 F1 C1 F2 C1 F3 SADI_TFA C1 C2 DANG_2 2.16 F1 F2 F2 F3 DANG_2 2.35 O2 C2 DANG_2 2.37 F1 C1 FLAT_TFA C1 C2 O1 O2 DANG_2 2.39 F3 C1 DANG_2 2.38 O1 C2 SADI_TFA 0.04 O1 O2 DFIX_2 1.55 C1 C2 DFIX_2 1.24 O2 C1 DFIX_2 1.34 F1 C2 F3 C2 DFIX_2 1.33 F2 C2 DFIX_2 1.25 O1 C1 DFIX_3 1.46 N1 C3 DFIX_3 1.22 C1 O1 DANG_3 2.45 C1 C3 RIGU_3 C1 O1 N1 C2 C3 DFIX_3 1.45 N1 C2 DANG_3 2.46 C1 C2 DFIX_3 1.36 C1 N1 FLAT_DMF C1 O1 N1 C2 C3 SADI_DMF C1 O1 SIMU 0.04 0.08 1 DFIX_4 1.45 N1 C2 SADI_DMF 0.04 C2 C3 DFIX_4 1.46 N1 C3 SADI_DMF N1 C1 DFIX_4 1.22 C1 O1 SADI_DMF 0.04 C1 C2 DFIX_4 1.36 C1 N1 SADI_DMF N1 C2 N1 C3 SADI_DMF 0.04 C1 C3 RIGU_4 C1 O1 N1 C2 C3 DANG_4 2.46 C1 C2 DANG_4 2.45 C1 C3 L.S. 10 PLAN 20 TEMP -173 CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 4 0 10 OMIT 5 0 16 OMIT 6 0 16 OMIT 5 0 24 REM REM REM WGHT 0.020500 8.909699 FVAR 0.16455 0.73447 0.65489 0.74225 0.77169 BI 3 0.628192 0.302993 0.641342 11.00000 0.01657 0.01272 = 0.02097 0.00179 0.00509 0.00175 O3 6 0.472900 0.314030 0.531682 11.00000 0.03730 0.03564 = 0.03017 -0.00213 -0.00454 0.01230 O2 6 0.571690 0.118690 0.527912 11.00000 0.07924 0.05433 = 0.02497 -0.00696 -0.00518 0.03268 PART 1 O1 6 0.730999 0.229065 0.516855 21.00000 0.03002 0.02469 = 0.02727 -0.00298 0.00640 -0.00288 PART 2 O1B 6 0.803338 0.218783 0.495441 -21.00000 0.02173 0.01591 = 0.06889 -0.01280 -0.01055 0.01011 PART 0 O6 6 0.602053 0.313712 0.741918 11.00000 0.02009 0.01955 = 0.02195 -0.00064 0.00367 0.00171 O7 6 0.647867 0.263918 0.837416 11.00000 0.02846 0.03177 = 0.02374 0.00589 0.00559 0.00248 O4 6 0.659212 0.127420 0.658192 11.00000 0.02388 0.01085 = 0.02889 0.00318 0.00417 0.00224 O5 6 0.602501 -0.038953 0.654696 11.00000 0.03231 0.01459 = 0.04265 0.00057 0.00131 -0.00011 N3 5 0.807606 0.384276 0.594196 11.00000 0.02221 0.01494 = 0.02371 0.00099 0.00778 0.00146 N2 5 0.657973 0.507032 0.654970 11.00000 0.02624 0.01092 = 0.02297 -0.00127 0.00549 0.00118 N1 5 0.459854 0.423360 0.650773 11.00000 0.02182 0.01825 = 0.02693 -0.00045 0.00519 0.00227 N5 5 0.785823 0.285211 0.701873 11.00000 0.01865 0.01255 = 0.02509 0.00084 0.00196 0.00127 N4 5 0.473200 0.203069 0.660286 11.00000 0.01985 0.02053 = 0.02040 0.00079 0.00345 -0.00162 C7 1 0.832295 0.484458 0.626320 11.00000 0.02704 0.01446 = 0.02999 0.00108 0.00595 -0.00232 AFIX 23 H7A 2 0.879911 0.524443 0.601122 11.00000 -1.20000 H7B 2 0.866300 0.468044 0.666528 11.00000 -1.20000 AFIX 0 C6 1 0.743373 0.553325 0.637994 11.00000 0.02887 0.01448 = 0.02373 0.00112 0.00336 -0.00014 C5 1 0.754272 0.662385 0.636441 11.00000 0.03103 0.01865 = 0.02935 0.00082 0.00192 -0.00485 AFIX 43 H5 2 0.814962 0.693466 0.623853 11.00000 -1.20000 AFIX 0 C4 1 0.674408 0.724979 0.653714 11.00000 0.04595 0.00994 = 0.03294 -0.00201 0.00230 0.00000 AFIX 43 H4 2 0.680182 0.799643 0.653452 11.00000 -1.20000 AFIX 0 C3 1 0.586806 0.677835 0.671218 11.00000 0.03513 0.01864 = 0.02977 -0.00326 0.00502 0.00775 AFIX 43 H3 2 0.531497 0.719396 0.683045 11.00000 -1.20000 AFIX 0 C2 1 0.580920 0.568489 0.671238 11.00000 0.02654 0.01951 = 0.02098 -0.00136 0.00264 0.00511 C1 1 0.488965 0.512198 0.692153 11.00000 0.02986 0.01842 = 0.03195 -0.00285 0.00891 0.00593 AFIX 23 H1A 2 0.501429 0.484954 0.734665 11.00000 -1.20000 H1B 2 0.432955 0.563044 0.693517 11.00000 -1.20000 AFIX 0 C15 1 0.427675 0.466124 0.589571 11.00000 0.03063 0.02687 = 0.03486 0.00416 0.00069 0.01005 AFIX 23 H15A 2 0.484104 0.505330 0.571931 11.00000 -1.20000 H15B 2 0.372507 0.516814 0.595416 11.00000 -1.20000 AFIX 0 C14 1 0.393179 0.383080 0.543945 11.00000 0.03004 0.03758 = 0.03237 0.00348 -0.00528 0.00481 AFIX 23 H14A 2 0.337006 0.342827 0.561113 11.00000 -1.20000 H14B 2 0.369242 0.417013 0.504951 11.00000 -1.20000 AFIX 0 C13 1 0.433184 0.219078 0.501573 11.00000 0.04429 0.04155 = 0.03555 -0.00317 -0.00474 -0.00398 AFIX 23 H13A 2 0.397005 0.175987 0.531876 11.00000 -1.20000 H13B 2 0.385637 0.238780 0.467508 11.00000 -1.20000 AFIX 0 C12 1 0.514894 0.158942 0.477220 11.00000 0.05065 0.04049 = 0.02990 -0.00608 -0.00927 -0.00130 AFIX 23 H12A 2 0.488750 0.100420 0.451066 11.00000 -1.20000 H12B 2 0.556975 0.204656 0.451514 11.00000 -1.20000 AFIX 0 C11 1 0.659670 0.064343 0.509959 11.00000 0.07620 0.03150 = 0.03069 -0.00901 -0.00364 0.01998 AFIX 23 H11A 2 0.640162 0.005427 0.482041 11.00000 -1.20000 H11B 2 0.693152 0.033764 0.547325 11.00000 -1.20000 AFIX 0 C10 1 0.731933 0.133661 0.477880 11.00000 0.06939 0.02589 = 0.05391 -0.00391 -0.02129 -0.00072 PART 1 AFIX 23 H10A 2 0.799335 0.101586 0.477485 21.00000 -1.20000 H10B 2 0.709005 0.149148 0.434807 21.00000 -1.20000 AFIX 23 PART 2 H10C 2 0.774426 0.082479 0.456189 -21.00000 -1.20000 H10D 2 0.689895 0.166856 0.444784 -21.00000 -1.20000 AFIX 0 PART 0 C9 1 0.784406 0.308354 0.488590 11.00000 0.08721 0.03399 = 0.02611 0.00189 0.00794 -0.01767 PART 1 AFIX 23 H9AA 2 0.749391 0.327911 0.449203 21.00000 -1.20000 H9AB 2 0.851106 0.280783 0.478360 21.00000 -1.20000 AFIX 23 PART 2 H9BC 2 0.712026 0.308171 0.477729 -21.00000 -1.20000 H9BD 2 0.817797 0.326762 0.449740 -21.00000 -1.20000 AFIX 0 PART 0 C8 1 0.797431 0.403360 0.526843 11.00000 0.03763 0.02226 = 0.02809 0.00536 0.00646 0.00104 AFIX 23 H8A 2 0.739330 0.450283 0.518943 11.00000 -1.20000 H8B 2 0.857693 0.441234 0.513372 11.00000 -1.20000 AFIX 0 C23 1 0.885286 0.306532 0.610819 11.00000 0.02085 0.01734 = 0.02993 0.00174 0.00791 0.00061 AFIX 23 H23A 2 0.952175 0.336721 0.603712 11.00000 -1.20000 H23B 2 0.876913 0.242957 0.584557 11.00000 -1.20000 AFIX 0 C24 1 0.876865 0.277047 0.678126 11.00000 0.01898 0.01223 = 0.02893 -0.00105 0.00439 -0.00184 C25 1 0.958287 0.244842 0.714988 11.00000 0.01766 0.02116 = 0.03684 0.00131 0.00451 0.00308 AFIX 43 H25 2 1.022662 0.238832 0.697966 11.00000 -1.20000 AFIX 0 C26 1 0.944335 0.221762 0.776541 11.00000 0.02255 0.03088 = 0.04306 0.00462 -0.00430 0.00415 AFIX 43 H26 2 0.998962 0.198501 0.802127 11.00000 -1.20000 AFIX 0 C27 1 0.849861 0.232681 0.801056 11.00000 0.02875 0.02610 = 0.02875 0.00400 0.00266 0.00088 AFIX 43 H27 2 0.838960 0.218801 0.843569 11.00000 -1.20000 AFIX 0 C28 1 0.772554 0.264334 0.761561 11.00000 0.02104 0.01320 = 0.02696 0.00161 0.00447 0.00145 C29 1 0.667298 0.280341 0.783315 11.00000 0.02300 0.01250 = 0.02899 0.00001 0.00528 -0.00161 C16 1 0.378492 0.362987 0.679558 11.00000 0.02042 0.02650 = 0.03670 -0.00164 0.01044 0.00542 AFIX 23 H16A 2 0.313481 0.390205 0.663387 11.00000 -1.20000 H16B 2 0.381626 0.375496 0.724845 11.00000 -1.20000 AFIX 0 C17 1 0.382636 0.245453 0.667919 11.00000 0.02005 0.02848 = 0.02716 -0.00219 0.00563 -0.00033 C18 1 0.298783 0.183024 0.670033 11.00000 0.01938 0.03959 = 0.04077 -0.00426 0.00730 -0.00326 AFIX 43 H18 2 0.234932 0.214238 0.674684 11.00000 -1.20000 AFIX 0 C19 1 0.307701 0.074555 0.665363 11.00000 0.02715 0.03508 = 0.04218 -0.00444 0.00786 -0.01427 AFIX 43 H19 2 0.250200 0.030803 0.666705 11.00000 -1.20000 AFIX 0 C20 1 0.401524 0.030628 0.658709 11.00000 0.03165 0.02429 = 0.02822 -0.00139 0.00431 -0.00687 AFIX 43 H20 2 0.409610 -0.043560 0.655360 11.00000 -1.20000 AFIX 0 C21 1 0.483556 0.097673 0.657047 11.00000 0.02450 0.02059 = 0.01909 0.00259 0.00366 -0.00157 C22 1 0.589111 0.056622 0.655631 11.00000 0.02920 0.01461 = 0.01799 0.00237 -0.00120 -0.00063 PART 1 O8A 6 -0.082278 0.456697 0.393678 51.00000 0.05317 0.05482 = 0.04058 -0.01380 0.01719 -0.02386 PART 2 O8B 6 -0.136649 0.533978 0.384720 -51.00000 0.02646 0.16589 = 0.04102 0.03800 0.01037 -0.00333 RESI TFA 1 SAME_2 0.02 0.02 O2 O1 C1 C2 F2 F3 F1 PART 1 O2 6 0.146625 0.339871 0.577705 31.00000 0.02685 0.07377 = 0.15229 -0.05293 0.00118 0.00625 O1 6 0.062127 0.353443 0.482965 31.00000 0.06325 0.07335 = 0.13387 0.06324 0.02788 -0.00263 C1 1 0.106276 0.307136 0.528878 31.00000 0.03320 0.03996 = 0.09189 -0.00944 0.03648 -0.00820 C2 1 0.109249 0.184719 0.524542 31.00000 0.04274 0.03783 = 0.04323 -0.00813 0.00863 -0.00333 F1 4 0.116846 0.136287 0.578408 31.00000 0.25764 0.09259 = 0.08599 0.03519 -0.06646 -0.09451 F3 4 0.185632 0.153154 0.492649 31.00000 0.03906 0.07706 = 0.19115 -0.03020 0.02915 0.02528 F2 4 0.028528 0.145942 0.498332 31.00000 0.04395 0.04831 = 0.13158 -0.03520 -0.00748 0.00233 RESI TFA 2 PART 2 O2 6 0.115760 0.360332 0.513880 -31.00000 0.10052 0.04609 = 0.10226 -0.01113 0.00230 -0.03172 O1 6 0.016704 0.298785 0.430895 -31.00000 0.11810 0.08477 = 0.05685 -0.02996 0.05239 -0.07034 C1 1 0.068206 0.291214 0.482187 -31.00000 0.08208 0.04506 = 0.07224 -0.02688 0.05456 -0.02866 C2 1 0.091242 0.182429 0.511993 -31.00000 0.07369 0.05201 = 0.07918 -0.03341 0.01814 -0.00494 F2 4 0.175717 0.141909 0.492935 -31.00000 0.07246 0.09382 = 0.17068 -0.06841 0.02844 0.00179 F3 4 0.102736 0.180296 0.573915 -31.00000 0.08857 0.19495 = 0.07950 -0.02500 -0.02295 0.10820 F1 4 0.021305 0.113500 0.499536 -31.00000 0.08274 0.04256 = 0.09480 0.01665 0.02081 -0.00992 RESI DMF 3 SAME_4 0.02 0.02 O1 C1 N1 C3 C2 PART 1 O1 6 -0.095334 0.511795 0.774164 41.00000 0.03084 0.04542 = 0.05505 -0.00547 0.01408 0.00504 C1 1 -0.010174 0.492017 0.758048 41.00000 0.02549 0.02396 = 0.03181 -0.00166 0.00124 -0.00235 AFIX 43 H1 2 0.000804 0.492991 0.714776 41.00000 -1.20000 AFIX 0 N1 5 0.068654 0.469267 0.795080 41.00000 0.04249 0.03358 = 0.04403 -0.00392 -0.01633 0.00322 C3 1 0.059191 0.461586 0.861089 41.00000 0.15537 0.08598 = 0.03610 -0.01139 -0.03835 0.02205 AFIX 137 H3A 2 -0.005340 0.490862 0.872741 41.00000 -1.50000 H3B 2 0.113329 0.501263 0.881889 41.00000 -1.50000 H3C 2 0.063135 0.387396 0.873635 41.00000 -1.50000 AFIX 0 C2 1 0.164848 0.446793 0.768560 41.00000 0.03049 0.04964 = 0.11739 -0.01394 -0.02062 0.00583 AFIX 137 H2A 2 0.183886 0.373720 0.777806 41.00000 -1.50000 H2B 2 0.215430 0.494678 0.786436 41.00000 -1.50000 H2C 2 0.160104 0.456824 0.723552 41.00000 -1.50000 AFIX 0 RESI DMF 4 PART 2 O1 6 -0.089691 0.490014 0.774536 -41.00000 0.03502 0.03658 = 0.03867 -0.00595 0.00036 0.00646 C1 1 -0.030902 0.488777 0.819369 -41.00000 0.03538 0.03348 = 0.03149 -0.00707 0.00401 -0.00604 AFIX 43 H1 2 -0.058159 0.500079 0.858952 -41.00000 -1.20000 AFIX 0 N1 5 0.067888 0.473022 0.817763 -41.00000 0.03126 0.02840 = 0.03283 0.00516 0.00541 -0.00956 C3 1 0.116603 0.456010 0.759382 -41.00000 0.04350 0.04242 = 0.04180 0.00793 0.01430 -0.00467 AFIX 137 H3A 2 0.066591 0.457895 0.725300 -41.00000 -1.50000 H3B 2 0.149802 0.387126 0.760130 -41.00000 -1.50000 H3C 2 0.166287 0.511531 0.753322 -41.00000 -1.50000 AFIX 0 C2 1 0.130120 0.474670 0.873707 -41.00000 0.05208 0.04987 = 0.04266 0.00825 -0.01009 -0.00736 AFIX 137 H2A 2 0.090314 0.497612 0.908610 -41.00000 -1.50000 H2B 2 0.185779 0.523746 0.868452 -41.00000 -1.50000 H2C 2 0.156429 0.403769 0.881960 -41.00000 -1.50000 AFIX 0 HKLF 4 REM rah20_abs_a.res in P2(1)/c REM R1 = 0.0271 for 6805 Fo > 4sig(Fo) and 0.0379 for all 8065 data REM 630 parameters refined using 324 restraints END WGHT 0.0205 8.9098 REM Highest difference peak 1.052, deepest hole -0.793, 1-sigma level 0.113 Q1 1 0.6816 0.3039 0.6790 11.00000 0.05 1.05 Q2 1 0.1410 0.2980 0.6185 11.00000 0.05 0.90 Q3 1 -0.0336 0.3203 0.4140 11.00000 0.05 0.88 Q4 1 0.5761 0.3022 0.6004 11.00000 0.05 0.87 Q5 1 0.6204 0.1578 0.5239 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0.43 6.29 10 -9 -3 4.03 6.77 10 -9 -3 11.57 7.68 10 9 -3 9.75 7.05 -10 -9 2 17.59 8.23 -10 9 2 11.96 8.19 -10 9 2 23.31 8.62 10 -9 -2 15.00 6.09 10 9 -2 19.85 6.52 10 -9 -2 6.88 6.75 10 -9 -2 14.68 7.77 10 9 -2 14.61 6.88 -10 9 1 18.80 8.86 -10 -9 1 24.53 8.70 -10 9 1 29.65 8.76 -10 9 1 25.04 9.09 10 -9 -1 27.46 6.28 10 9 -1 36.80 6.82 10 -9 -1 42.12 7.57 10 -9 -1 28.39 8.14 10 9 -1 31.47 7.45 -10 9 0 384.13 20.60 -10 -9 0 406.12 20.72 -10 9 0 371.50 20.25 -10 9 0 441.59 20.79 10 -9 0 355.01 17.24 10 9 0 404.19 17.88 10 -9 0 404.25 18.34 10 -9 0 402.01 19.15 10 9 0 391.47 18.26 -10 9 -1 21.89 8.68 -10 -9 -1 20.20 8.46 -10 9 -1 31.27 9.24 -10 9 -1 19.79 8.39 10 -9 1 9.61 5.76 10 9 1 5.88 6.14 10 -9 1 9.50 6.08 10 -9 1 14.53 7.33 10 9 1 15.57 5.98 -10 9 -2 126.54 12.16 -10 -9 -2 140.28 12.08 -10 9 -2 133.90 12.11 -10 9 -2 139.91 12.20 10 -9 2 137.17 9.44 10 9 2 118.36 9.43 10 -9 2 136.98 9.72 10 -9 2 127.97 10.61 10 9 2 137.45 9.75 10 9 3 8.75 7.06 -10 9 -3 29.82 9.02 -10 -9 -3 12.53 8.00 -10 9 -3 26.35 8.67 -10 9 -3 10.27 8.55 10 -9 3 20.77 6.11 10 9 3 20.38 6.43 10 -9 3 17.15 6.60 10 -9 3 24.74 7.72 10 9 3 22.24 6.15 -10 -9 -4 259.90 15.81 10 9 4 257.27 12.79 -10 9 -4 235.96 15.18 10 -9 4 236.97 12.98 10 9 4 239.13 13.14 10 -9 4 242.97 13.09 10 -9 4 266.20 14.16 10 9 4 248.77 14.97 -10 9 -4 223.28 15.39 10 9 5 11.69 7.28 10 9 5 22.47 5.82 -10 9 -5 20.43 8.44 10 -9 5 32.41 7.03 10 9 5 20.30 6.95 10 -9 5 26.39 6.46 10 -9 5 37.06 7.71 -10 9 -5 19.41 8.23 10 9 6 197.38 10.96 -10 9 -6 225.92 14.23 10 -9 6 211.06 11.86 10 -9 6 238.93 13.17 10 9 6 217.42 13.98 -10 9 -6 203.86 14.25 -10 9 -7 10.19 8.18 -10 9 -7 13.00 8.78 -10 9 -7 7.69 8.27 10 9 7 6.10 7.10 -10 -9 -7 3.76 6.75 -10 9 -7 4.89 6.62 10 -9 7 8.08 6.07 10 -9 7 12.77 7.06 10 9 7 10.97 5.10 10 9 8 34.58 5.26 -10 9 -8 25.70 8.30 10 9 8 44.43 8.92 -10 9 -8 48.57 7.66 10 -9 8 47.39 6.68 -10 -9 -8 43.25 7.53 10 -9 8 40.93 7.70 -10 9 -8 36.90 9.35 -10 9 -9 26.42 8.29 10 9 9 27.62 8.70 -10 -9 -9 33.16 7.57 -10 9 -9 36.29 7.50 10 9 9 28.20 5.03 -10 9 -9 26.39 8.67 -10 9 -10 308.50 15.69 10 9 10 306.78 17.26 -10 -9 -10 284.37 14.53 -10 9 -10 289.82 14.49 -10 9 -10 266.26 16.19 -10 -9 -11 -0.54 3.86 10 9 11 15.60 8.47 -10 9 -11 -9.13 7.68 -10 -9 -11 2.28 7.14 -10 9 -11 4.82 6.77 -10 9 -11 -2.53 7.98 10 9 12 14.47 9.02 -10 9 -12 -3.88 7.27 -10 -9 -12 3.72 7.26 -10 9 -12 4.02 7.24 -10 9 -12 -3.07 8.42 -10 -9 -13 -9.10 7.93 -10 9 -13 -9.65 7.81 -10 9 -13 -0.92 7.31 10 9 13 7.03 9.64 -10 -9 -14 238.22 14.20 -10 9 -14 243.43 13.89 10 9 14 265.19 16.84 10 9 15 -9.00 9.78 -10 9 -15 -2.88 6.80 10 -10 -15 40.55 9.96 10 10 -15 31.69 10.96 -10 10 15 22.14 10.18 -10 -10 14 34.60 7.27 10 -10 -14 51.84 9.83 10 10 -14 43.58 10.81 -10 10 14 23.38 10.26 -10 -10 13 -0.75 6.49 10 10 -13 3.86 9.51 -10 10 13 -11.18 10.37 -10 -10 12 265.39 13.59 10 10 -12 286.98 17.69 -10 10 12 255.70 17.04 -10 -10 11 12.39 6.56 10 10 -11 16.86 9.45 -10 10 11 2.92 8.98 10 -10 -10 206.69 14.00 -10 10 10 194.43 14.81 -10 -10 10 196.22 9.90 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8.57 10 10 -3 2.30 7.11 -10 10 2 327.18 19.98 -10 -10 2 377.67 19.85 -10 10 2 347.39 19.35 -10 10 2 345.74 19.33 10 -10 -2 338.73 16.01 10 10 -2 360.82 16.50 10 -10 -2 343.59 17.40 10 -10 -2 345.37 18.45 10 10 -2 342.07 17.52 -10 10 1 24.05 9.32 -10 -10 1 14.01 8.54 -10 10 1 21.01 8.95 -10 10 1 21.51 9.19 10 -10 -1 23.25 6.47 10 10 -1 20.59 6.50 10 -10 -1 22.74 7.39 10 -10 -1 23.05 8.74 10 10 -1 26.49 7.20 -10 10 0 3.95 9.09 -10 -10 0 -11.76 8.42 -10 10 0 1.45 8.35 -10 10 0 -7.06 9.38 10 -10 0 -1.52 5.78 10 10 0 -0.41 6.12 10 -10 0 5.90 6.76 10 -10 0 -5.82 8.25 10 10 0 9.62 6.80 -10 10 -1 2.34 8.43 -10 -10 -1 5.14 8.31 -10 10 -1 8.71 8.27 -10 10 -1 6.26 9.05 10 -10 1 8.09 5.85 10 10 1 7.39 6.25 10 -10 1 5.25 6.72 10 -10 1 8.59 8.14 10 10 1 5.30 6.66 -10 10 -2 345.22 19.69 -10 -10 -2 350.13 19.32 -10 10 -2 347.56 19.43 -10 10 -2 382.94 19.43 10 -10 2 354.77 16.31 10 10 2 371.33 16.78 10 -10 2 359.33 17.15 10 -10 2 336.19 18.10 10 10 2 341.25 16.81 -10 10 -3 -2.29 8.80 -10 10 -3 8.78 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169.83 13.83 -10 -10 -9 6.82 7.07 -10 10 -9 6.09 6.65 10 -10 9 3.75 6.02 -10 10 -9 3.99 8.44 -10 10 -9 -0.70 8.68 10 10 9 4.44 8.18 -10 10 -10 20.23 8.49 -10 -10 -10 16.49 7.61 -10 10 -10 15.73 7.21 -10 10 -10 8.23 8.46 10 10 10 18.14 9.22 10 10 11 3.87 8.81 -10 -10 -11 3.55 7.38 -10 10 -11 5.08 6.79 -10 10 -11 7.34 7.73 -10 10 -12 197.17 12.29 -10 -10 -12 208.59 12.83 10 10 12 186.74 15.05 -10 10 -12 187.61 12.70 -10 10 -13 10.42 8.03 10 10 13 -1.62 9.39 -10 -10 -13 6.60 7.99 -10 10 -13 7.63 7.68 10 10 14 5.80 9.91 -10 10 -14 -2.68 7.28 -10 -11 12 74.77 8.19 10 11 -12 48.97 10.98 -10 11 12 44.29 10.52 10 -11 -11 5.26 8.66 10 11 -11 2.31 9.52 -10 11 11 0.75 9.87 -10 11 10 128.20 13.29 10 11 -10 139.62 13.12 10 -11 -10 161.88 13.02 -10 11 9 70.77 11.83 10 -11 -9 101.37 10.72 10 -11 -9 89.59 8.87 10 11 -9 91.76 9.09 10 11 -9 76.74 11.02 -10 11 9 70.41 6.69 10 -11 -8 296.34 16.73 -10 11 8 285.96 17.60 -10 -11 8 312.76 14.01 10 11 -8 310.17 17.65 10 11 -8 294.34 14.81 10 -11 -8 305.95 14.81 -10 11 7 18.42 4.05 -10 11 7 8.81 8.87 -10 -11 7 4.61 6.95 10 11 -7 23.71 6.98 10 11 -7 8.28 9.11 10 -11 -7 13.25 6.67 10 -11 -7 22.15 8.80 -10 11 6 2.93 9.15 -10 -11 6 3.88 7.67 10 11 -6 1.61 6.49 10 -11 -6 16.88 6.60 10 11 -6 10.70 8.29 10 -11 -6 24.71 8.95 -10 11 5 65.32 10.67 10 -11 -5 74.28 10.27 -10 -11 5 67.74 9.36 10 -11 -5 73.53 7.85 10 11 -5 78.96 10.55 10 11 -5 75.63 8.06 -10 11 4 313.73 19.11 10 -11 -4 345.77 17.97 10 11 -4 299.99 17.81 10 -11 -4 352.48 19.40 10 -11 -4 359.56 15.92 10 11 -4 355.17 16.35 -10 11 3 24.27 9.63 10 -11 -3 25.81 8.66 10 -11 -3 34.30 6.66 10 11 -3 37.97 7.09 10 -11 -3 31.13 9.99 10 11 -3 35.51 8.45 -10 11 2 2.21 9.03 10 -11 -2 -4.38 7.69 10 -11 -2 -10.54 6.49 10 11 -2 -4.75 6.61 10 -11 -2 -8.50 9.43 10 11 -2 4.05 7.83 10 -11 -1 59.03 8.95 10 -11 -1 58.03 7.39 10 11 -1 45.25 7.58 10 -11 -1 41.28 10.12 10 11 -1 45.39 8.30 10 -11 0 245.52 12.82 10 11 0 283.08 13.73 10 -11 0 238.94 14.38 10 11 0 226.41 14.03 10 -11 0 270.76 16.25 -10 11 0 218.89 16.41 10 -11 1 118.07 10.34 10 -11 1 116.00 8.98 10 11 1 131.42 9.50 10 11 1 124.26 10.33 10 -11 1 132.04 12.16 -10 11 -1 135.23 13.13 -10 11 -2 47.33 10.19 10 -11 2 25.44 6.69 10 11 2 42.34 7.23 10 -11 2 37.61 7.93 10 -11 2 33.76 9.33 10 11 2 33.55 7.70 -10 11 -3 7.74 9.36 10 -11 3 10.42 7.15 10 11 3 3.23 6.41 10 -11 3 0.38 6.37 10 -11 3 -3.02 8.88 10 11 3 3.54 6.41 10 -11 4 186.52 11.07 10 11 4 199.31 11.43 10 -11 4 155.56 11.41 -10 -11 -4 197.16 11.21 -10 11 -4 178.08 10.86 10 11 4 157.31 10.82 -10 11 -4 175.54 14.14 10 -11 5 66.55 8.32 -10 -11 -5 63.40 7.86 -10 11 -5 66.83 8.06 10 -11 5 64.16 7.83 10 11 5 62.18 7.95 10 11 5 45.46 7.13 -10 11 -5 85.48 11.20 -10 11 -6 101.30 11.70 -10 11 -6 114.81 9.06 -10 -11 -6 108.89 9.17 10 -11 6 97.58 9.22 10 -11 6 109.71 9.24 10 11 6 106.89 9.38 -10 -11 -7 3.52 6.62 -10 11 -7 5.60 6.64 10 -11 7 13.42 6.58 -10 11 -7 2.52 8.68 10 -11 7 0.43 6.87 10 11 7 2.60 6.98 -10 -11 -8 61.04 8.20 10 -11 8 53.20 7.88 -10 11 -8 67.65 10.25 -10 11 -8 61.79 7.96 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6.46 11 0 -6 598.42 25.04 -11 0 6 607.60 24.33 -11 0 6 589.83 24.53 -11 0 5 -0.88 5.72 -11 0 5 2.07 4.86 11 0 -5 -0.49 5.32 -11 0 4 345.65 16.26 -11 0 4 332.33 15.64 11 0 -4 358.18 16.64 -11 0 3 -1.72 5.54 -11 0 3 4.42 4.98 11 0 -3 -3.41 5.57 -11 0 2 30.15 6.24 -11 0 2 36.07 5.86 11 0 -2 42.98 6.31 -11 0 1 -6.73 5.77 11 0 -1 1.94 5.35 -11 0 1 1.60 4.73 11 0 0 342.40 16.47 -11 0 0 353.02 15.84 11 0 1 -7.39 6.06 -11 0 -1 -3.65 4.97 -11 0 -2 102.72 8.11 -11 0 -2 89.62 6.82 -11 0 -3 -5.61 4.97 -11 0 -3 2.45 5.36 -11 0 -3 1.23 5.08 -11 0 -4 399.15 17.24 -11 0 -4 431.54 18.18 -11 0 -4 405.21 18.00 -11 0 -5 4.05 5.51 -11 0 -5 -3.45 4.79 11 0 5 4.60 4.47 -11 0 -6 -3.26 4.90 -11 0 -6 10.48 5.74 11 0 6 5.14 4.43 -11 0 -7 8.76 5.48 -11 0 -7 -6.42 5.78 11 0 7 2.66 4.78 -11 0 -8 212.07 11.58 -11 0 -8 219.09 11.71 11 0 8 199.55 11.13 -11 0 -9 0.80 5.30 11 0 9 3.26 4.98 -11 0 -9 -2.52 5.82 -11 0 -9 1.06 6.12 -11 0 -10 61.64 6.96 11 0 10 47.42 6.53 -11 0 -10 56.78 7.43 -11 0 -10 51.25 7.65 -11 0 -11 3.70 6.80 -11 0 -11 3.97 5.62 11 0 11 3.09 5.46 -11 0 -11 -5.08 6.35 -11 0 -11 3.20 6.42 -11 0 -12 208.86 13.52 -11 0 -12 261.72 12.64 11 0 12 234.97 12.83 -11 0 -12 235.60 13.35 -11 0 -12 212.48 13.43 -11 0 -13 -1.10 7.39 -11 0 -13 8.69 5.89 11 0 13 3.81 5.85 -11 0 -13 16.73 7.26 -11 0 -13 2.09 6.71 -11 0 -14 129.16 9.08 -11 0 -14 119.40 10.67 11 0 14 118.29 9.49 -11 0 -14 111.00 10.19 -11 0 -14 118.28 10.19 -11 0 -15 -5.72 8.03 -11 0 -15 0.39 5.98 11 0 15 10.29 6.72 -11 0 -15 1.67 7.09 -11 0 -15 0.51 6.79 -11 0 -16 60.97 8.30 -11 0 -16 49.17 5.70 -11 0 -16 74.33 9.61 11 0 16 63.34 8.60 -11 0 -16 73.23 7.82 -11 0 -17 -0.24 4.40 -11 0 -17 10.29 8.23 11 0 17 10.03 7.30 -11 0 -17 -3.48 6.31 -11 0 -18 256.67 14.83 11 0 18 228.12 13.68 -11 0 -18 260.67 12.38 -11 0 -19 -2.00 2.87 -11 0 -19 3.81 6.66 11 0 19 -0.60 7.75 -11 0 -19 8.54 8.72 -11 0 -20 6.79 6.68 -11 0 -20 8.18 9.33 11 0 20 2.49 7.96 -11 -1 21 5.81 7.98 -11 1 21 16.63 8.84 11 1 -21 17.52 9.56 11 -1 -21 11.89 4.57 -11 -1 20 64.51 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193.87 14.47 -11 8 0 196.58 14.26 -11 8 0 223.83 14.89 11 -8 0 187.76 11.77 11 8 0 197.07 12.17 11 -8 0 198.38 11.77 11 -8 0 207.44 12.15 11 8 0 184.24 11.97 -11 8 -1 13.05 8.59 -11 8 -1 5.98 8.71 -11 8 -1 12.61 9.10 11 -8 1 -2.72 6.56 11 8 1 -1.39 6.62 11 -8 1 6.75 5.93 11 -8 1 7.10 6.26 11 8 1 7.49 5.95 11 8 2 37.72 6.93 -11 8 -2 60.16 10.32 11 -8 2 40.34 7.66 11 8 2 38.67 7.56 11 -8 2 54.10 7.18 11 -8 2 67.18 7.88 -11 8 -2 51.18 9.51 11 8 3 147.93 10.05 -11 8 -3 150.77 12.95 11 -8 3 168.73 11.04 11 8 3 151.44 10.92 11 -8 3 152.92 10.39 11 -8 3 170.36 10.61 -11 8 -3 127.97 12.31 11 8 4 288.37 14.90 -11 8 -4 337.81 18.39 11 -8 4 322.53 16.14 11 8 4 334.53 16.23 11 -8 4 291.68 15.15 11 -8 4 331.31 15.80 -11 8 -4 308.81 17.73 11 8 4 347.13 17.54 -11 8 -5 53.95 9.75 11 8 5 86.00 9.60 -11 8 -5 61.34 10.67 -11 8 -5 70.33 11.04 11 -8 5 73.19 8.70 11 8 5 48.63 8.24 11 -8 5 59.69 7.79 11 -8 5 71.85 8.13 11 8 5 74.27 7.37 -11 8 -6 1.35 8.07 -11 8 -6 -5.46 8.77 -11 8 -6 -8.22 8.58 11 8 6 -0.65 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1.26 9.02 11 9 -14 28.41 10.09 -11 -9 14 41.88 7.71 11 -9 -14 43.21 9.67 11 9 -13 5.39 9.60 -11 -9 13 -3.25 7.01 11 -9 -13 8.06 8.67 11 9 -12 316.13 18.98 11 -9 -12 344.26 17.17 11 9 -12 329.37 17.30 -11 -9 12 308.16 15.71 11 9 -11 10.95 9.01 11 -9 -11 -0.51 7.54 11 9 -11 5.38 8.04 -11 -9 11 10.43 7.01 11 9 -10 -3.55 8.80 11 -9 -10 3.98 7.60 11 9 -10 0.52 7.67 -11 -9 10 2.95 6.71 11 9 -9 3.00 7.30 11 9 -9 1.38 8.31 11 -9 -9 -1.92 7.01 -11 -9 9 4.25 6.96 11 -9 -9 1.18 7.75 -11 9 8 513.36 25.46 11 -9 -8 526.48 24.02 -11 -9 8 545.32 19.65 11 9 -8 547.71 23.33 11 9 -8 484.79 24.38 11 -9 -8 531.30 23.02 11 -9 -7 9.15 6.64 11 9 -7 4.85 7.00 -11 9 7 -8.23 9.45 11 -9 -7 1.13 7.84 -11 -9 7 2.38 4.18 11 9 -7 3.26 7.93 11 -9 -6 55.39 7.82 11 9 -6 48.45 8.18 -11 9 6 51.71 10.79 11 -9 -6 44.96 8.25 11 -9 -6 40.31 8.71 -11 -9 6 45.24 5.67 11 9 -6 52.45 9.02 -11 9 5 -0.84 2.08 -11 9 5 -1.27 2.30 -11 9 5 -3.76 8.78 11 -9 -5 -0.45 6.68 11 9 -5 -3.33 7.03 11 -9 -5 -1.63 7.43 11 -9 -5 -13.42 8.54 -11 -9 5 -3.38 5.44 11 9 -5 -1.22 7.68 -11 9 4 289.53 17.58 -11 9 4 276.79 17.38 11 -9 -4 258.55 14.31 11 9 -4 289.32 15.09 11 -9 -4 294.30 15.37 11 -9 -4 274.44 15.66 11 9 -4 271.77 15.62 -11 -9 3 -3.00 8.14 -11 9 3 6.81 8.67 -11 9 3 4.46 9.25 11 -9 -3 -0.88 6.53 11 9 -3 -2.34 7.11 11 -9 -3 5.71 7.19 11 -9 -3 -1.05 8.02 11 9 -3 11.44 7.22 -11 9 2 201.52 15.48 -11 -9 2 196.62 14.71 -11 9 2 230.93 15.92 -11 9 2 204.37 15.13 11 -9 -2 206.77 12.37 11 9 -2 220.37 12.95 11 -9 -2 221.24 13.23 11 -9 -2 221.16 13.52 11 9 -2 231.10 13.43 -11 9 1 7.24 9.05 -11 -9 1 8.88 8.57 -11 9 1 9.92 8.87 -11 9 1 4.41 8.87 11 -9 -1 17.78 6.52 11 9 -1 9.16 6.77 11 -9 -1 14.32 6.87 11 -9 -1 19.35 7.73 11 9 -1 5.32 7.02 -11 9 0 123.11 12.50 -11 9 0 150.63 13.26 -11 9 0 136.36 12.75 11 -9 0 125.57 9.84 11 9 0 144.73 10.37 11 -9 0 135.42 10.35 11 -9 0 144.79 11.04 11 9 0 122.71 10.41 -11 9 -1 -2.33 9.04 -11 9 -1 17.61 9.35 -11 9 -1 12.30 8.93 11 -9 1 7.98 6.38 11 9 1 8.27 6.99 11 -9 1 15.51 6.76 11 -9 1 12.37 7.36 11 9 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359.61 16.35 -12 6 9 330.43 20.93 -12 6 8 58.97 11.53 -12 6 8 81.39 10.93 12 -6 -8 69.95 8.85 12 6 -8 70.12 9.22 -12 -6 8 89.26 8.79 12 -6 -8 57.70 7.09 -12 -6 8 77.43 9.87 -12 6 7 30.31 10.14 -12 6 7 37.46 9.15 12 -6 -7 33.25 7.69 -12 -6 7 40.13 7.72 12 -6 -7 24.73 7.29 12 6 -7 36.26 8.07 12 -6 -7 31.21 6.10 -12 -6 7 23.31 8.47 -12 6 6 -1.74 9.56 12 -6 -6 -0.51 6.75 12 6 -6 -2.14 6.98 12 -6 -6 0.33 5.37 -12 -6 6 -4.77 8.19 -12 6 6 -0.27 1.14 12 -6 -6 7.43 6.57 -12 -6 6 -0.46 6.70 12 -6 -5 293.46 15.51 12 6 -5 301.53 15.93 12 -6 -5 301.21 13.78 -12 -6 5 327.26 17.34 -12 6 5 260.93 12.44 12 -6 -5 299.61 15.27 -12 -6 5 331.08 15.51 12 -6 -4 67.93 8.37 12 6 -4 81.35 9.04 12 -6 -4 76.83 8.33 -12 -6 4 76.37 8.57 12 -6 -4 70.50 6.78 -12 -6 4 73.01 9.58 -12 6 4 65.15 5.54 -12 6 3 159.31 12.60 12 -6 -3 123.98 9.95 12 6 -3 148.72 10.48 12 -6 -3 125.70 9.49 12 -6 -3 151.19 8.32 -12 6 3 137.71 6.71 -12 -6 3 117.07 10.96 -12 6 2 -0.75 8.41 -12 6 2 -1.39 9.00 12 -6 -2 -2.50 6.87 12 6 -2 1.03 6.76 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13.85 12 7 12 157.63 13.16 -12 7 -12 149.09 12.28 -12 7 -12 143.07 13.37 12 7 13 53.56 5.30 12 7 13 60.09 10.24 -12 7 -13 74.98 9.88 -12 7 -13 44.66 10.00 12 7 14 5.96 3.96 -12 7 -14 2.25 8.63 -12 7 -14 0.57 7.84 12 7 14 6.83 9.13 -12 7 -15 48.33 9.55 -12 7 -15 33.60 8.74 12 7 15 65.09 11.09 -12 -8 14 215.25 13.10 12 -8 -14 214.55 14.63 12 -8 -14 235.66 14.88 12 8 -14 227.54 15.29 12 8 -14 190.10 15.74 -12 -8 13 42.06 8.31 12 -8 -13 46.25 9.64 12 8 -13 48.19 10.68 12 -8 -13 50.51 9.78 12 8 -13 45.00 9.97 12 -8 -12 87.81 10.64 -12 -8 12 97.60 9.83 12 8 -12 97.83 11.26 12 8 -12 100.86 12.22 12 -8 -12 97.03 10.84 -12 -8 11 -0.91 7.28 12 8 -11 -7.92 8.95 12 -8 -11 -1.63 8.11 12 8 -11 -1.71 8.04 -12 -8 10 177.42 11.94 12 8 -10 183.19 13.85 12 -8 -10 181.19 12.66 12 8 -10 194.53 13.29 -12 -8 9 85.24 8.96 12 8 -9 81.67 10.78 12 -8 -9 86.93 9.48 12 -8 -9 72.49 9.60 12 8 -9 92.94 10.21 -12 -8 8 270.05 14.60 12 -8 -8 282.25 15.75 12 -8 -8 286.21 15.05 12 -8 -8 260.80 14.85 12 8 -8 244.63 15.89 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342.91 19.49 -12 -8 0 343.51 18.89 -12 8 0 365.31 19.79 -12 8 0 349.30 19.69 12 -8 0 308.29 16.31 12 8 0 328.50 16.54 12 -8 0 300.82 15.98 12 -8 0 326.14 15.84 12 8 0 288.23 16.15 -12 -8 -1 53.77 10.07 12 8 1 44.66 8.40 -12 8 -1 31.18 10.72 12 -8 1 51.59 8.34 12 8 1 34.27 7.80 12 -8 1 52.49 7.82 12 -8 1 55.10 7.50 -12 8 -1 56.08 10.48 -12 -8 -2 32.42 9.38 12 8 2 46.02 7.49 -12 8 -2 51.76 11.19 12 -8 2 34.01 7.79 12 8 2 40.23 7.92 12 -8 2 55.78 7.77 12 -8 2 45.06 7.41 -12 8 -2 43.40 10.01 12 8 3 0.95 6.60 -12 8 -3 16.55 10.24 12 -8 3 5.10 7.15 12 8 3 -1.53 6.99 12 -8 3 11.42 6.75 12 -8 3 21.97 6.84 -12 8 -3 11.94 9.41 12 8 4 171.89 11.57 -12 8 -4 202.17 15.86 12 -8 4 180.88 12.42 12 8 4 193.49 12.54 12 -8 4 187.41 11.81 12 -8 4 212.16 11.99 -12 8 -4 211.31 15.11 12 8 5 67.48 7.92 12 -8 5 91.70 9.81 12 8 5 84.34 9.71 -12 8 -5 79.27 12.27 12 8 5 99.75 10.50 -12 8 -5 81.87 11.11 12 -8 6 244.13 14.23 12 8 6 220.99 13.74 -12 8 -6 194.09 15.90 -12 8 -6 224.72 15.49 12 8 6 197.66 14.11 12 8 6 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8.57 13 7 -12 1.86 8.84 13 -7 -12 -5.03 7.24 -13 -7 11 132.56 10.99 13 -7 -11 116.92 11.32 13 7 -11 125.98 11.75 13 7 -11 111.62 12.13 13 -7 -11 109.35 9.46 -13 -7 10 208.23 13.35 13 -7 -10 228.17 14.42 13 7 -10 231.23 14.60 13 7 -10 197.10 14.75 13 -7 -10 206.58 11.98 -13 -7 9 160.66 11.70 13 -7 -9 143.91 10.00 13 -7 -9 146.46 11.94 13 7 -9 151.45 12.40 13 7 -9 144.93 12.79 13 7 -8 6.67 8.43 13 -7 -8 14.42 8.10 -13 -7 8 15.90 7.59 13 -7 -8 8.26 7.54 13 7 -8 19.17 8.42 13 -7 -8 9.10 6.27 -13 7 8 13.88 5.13 13 7 -7 48.86 9.20 13 -7 -7 42.13 8.34 13 7 -7 28.79 8.60 13 -7 -7 39.12 6.86 -13 7 7 11.23 4.41 13 -7 -7 39.91 8.53 -13 -7 7 43.45 8.44 13 -7 -6 130.70 10.98 13 7 -6 143.49 11.64 13 -7 -6 139.97 9.36 -13 7 6 113.91 7.52 13 -7 -6 145.37 11.00 -13 -7 6 141.96 11.21 13 -7 -5 196.92 13.04 13 7 -5 186.38 13.03 13 -7 -5 222.01 11.22 -13 7 5 171.50 9.10 13 -7 -5 205.60 12.95 -13 -7 5 189.28 12.59 13 -7 -4 73.80 9.31 13 7 -4 71.29 9.51 13 -7 -4 86.46 7.54 -13 7 4 74.74 5.42 13 -7 -4 78.92 8.99 -13 -7 4 96.62 9.51 13 -7 -3 -0.51 6.89 13 -7 -3 -0.53 7.30 13 7 -3 -6.60 7.58 -13 -7 3 -7.28 2.21 13 -7 -3 2.44 5.42 13 -7 -2 63.81 8.42 13 -7 -2 71.62 9.13 13 7 -2 79.66 9.65 13 -7 -2 76.60 7.38 13 -7 -1 220.15 12.76 13 -7 -1 203.33 11.18 13 -7 -1 190.12 12.84 13 7 -1 203.28 13.47 -13 7 0 98.26 12.96 13 -7 0 92.85 9.87 13 7 0 97.95 10.47 13 -7 0 103.54 9.91 13 -7 0 116.07 8.30 -13 7 0 121.76 12.69 -13 7 -1 11.76 9.34 -13 7 -1 4.89 10.19 13 -7 1 26.11 8.10 13 7 1 16.96 8.21 -13 7 -2 19.11 9.62 -13 7 -2 17.35 10.31 13 -7 2 9.32 8.04 13 7 2 13.73 8.01 -13 7 -3 112.28 12.12 -13 7 -3 123.22 14.38 13 -7 3 128.75 11.01 13 7 3 107.24 10.68 -13 7 -4 220.97 15.33 -13 7 -4 173.46 16.26 13 -7 4 200.10 13.62 13 7 4 215.81 13.66 -13 7 -5 77.95 11.15 -13 7 -5 66.25 12.92 13 -7 5 80.57 9.94 13 7 5 70.63 9.64 -13 7 -6 1.74 11.27 -13 7 -6 12.79 8.93 13 7 6 20.43 8.06 13 -7 6 15.54 8.55 13 7 6 21.12 8.31 -13 7 -7 51.09 10.19 13 7 7 46.38 9.33 13 7 8 144.07 12.13 -13 7 -8 122.30 12.18 -13 7 -9 71.07 10.48 13 7 9 90.94 10.68 -13 7 -10 25.55 9.36 13 7 10 24.95 9.28 -13 7 -10 9.10 10.53 -13 7 -11 -5.94 9.13 13 7 11 12.36 9.07 -13 7 -11 5.78 11.06 -13 7 -12 24.46 9.58 -13 7 -12 22.67 10.89 13 7 12 25.21 9.47 13 -8 -12 181.73 13.50 13 -8 -12 176.38 13.13 13 8 -12 180.06 13.65 13 8 -12 149.20 14.00 13 -8 -11 9.73 7.71 13 8 -11 18.70 9.01 13 8 -11 34.63 10.31 13 -8 -11 26.34 9.18 13 -8 -10 -6.54 7.76 13 -8 -10 -2.80 8.13 13 8 -10 1.47 9.17 13 8 -10 0.59 8.55 13 -8 -9 35.20 8.73 13 8 -9 25.75 9.69 13 -8 -9 24.99 7.88 13 -8 -9 33.63 8.62 13 8 -9 34.38 9.20 13 8 -8 248.83 14.82 13 -8 -8 271.64 13.75 13 8 -8 262.98 14.03 13 -8 -8 289.81 14.37 13 -8 -8 266.31 12.47 13 8 -7 58.48 10.05 13 -8 -7 64.46 9.65 13 -8 -7 61.43 9.08 13 8 -7 48.45 9.59 13 -8 -7 37.80 7.72 -13 8 7 38.77 5.20 13 8 -6 49.86 9.63 13 -8 -6 46.51 8.24 13 -8 -6 39.56 8.78 13 8 -6 38.40 8.99 13 -8 -6 27.37 7.21 -13 8 6 33.78 4.64 13 8 -5 5.03 8.25 13 -8 -5 7.43 7.90 13 -8 -5 10.23 6.80 13 8 -5 11.69 8.31 13 -8 -5 18.71 8.21 13 -8 -4 148.84 11.84 13 8 -4 164.22 12.21 13 -8 -4 159.26 10.69 13 8 -4 158.78 12.70 13 -8 -4 184.99 12.14 13 -8 -3 88.76 9.80 13 8 -3 90.27 10.08 13 -8 -3 91.13 8.44 13 8 -3 93.86 10.46 13 -8 -3 118.15 10.35 13 -8 -2 120.89 10.80 13 8 -2 128.89 11.39 13 -8 -2 144.81 9.91 13 8 -2 121.62 11.35 13 -8 -2 142.32 11.18 13 -8 -1 12.59 7.26 13 8 -1 9.15 7.86 13 -8 -1 18.35 6.72 13 8 -1 7.13 7.62 13 -8 -1 18.53 7.39 13 -8 0 79.69 9.70 13 8 0 109.34 10.51 13 -8 0 104.77 8.76 13 8 0 84.58 9.77 13 -8 0 106.78 9.88 13 -8 1 60.68 9.06 13 8 1 63.88 9.42 13 -8 1 85.49 8.29 13 8 1 49.09 8.84 13 -8 1 60.71 8.44 13 -8 2 216.85 13.14 13 -8 2 250.63 12.85 13 -8 2 223.80 13.97 13 8 2 212.35 13.96 13 -8 3 15.92 8.17 13 8 3 15.79 8.08 13 -8 4 0.56 7.78 13 8 4 13.82 8.27 -13 8 -5 -0.89 11.41 13 8 5 0.48 6.96 13 -8 5 12.64 8.13 13 8 5 8.44 8.11 13 -8 6 306.49 16.60 13 8 6 266.53 15.72 13 8 6 236.53 14.18 13 8 6 282.96 16.67 -13 8 -6 284.21 20.09 13 -8 7 15.08 9.03 13 8 7 13.51 8.53 13 8 7 24.64 8.93 13 8 7 8.89 6.40 -13 8 -7 3.47 11.77 13 8 8 25.17 8.97 13 8 8 19.83 6.53 -13 8 -8 -1.67 11.43 13 8 9 32.17 6.41 13 8 9 34.41 9.35 -13 8 -9 22.51 9.87 -13 8 -9 24.01 11.12 13 8 10 101.92 8.33 -13 8 -10 138.33 12.90 13 8 10 139.50 12.90 -13 8 -10 112.87 13.70 13 8 11 17.95 5.45 -13 8 -11 28.05 9.81 13 8 11 36.50 10.08 -13 8 -11 31.70 11.21 13 -9 -10 255.97 15.25 13 9 -10 214.06 15.09 13 9 -10 222.95 16.59 13 -9 -10 244.17 14.58 13 -9 -9 -3.67 8.92 13 -9 -9 -3.91 8.50 13 9 -9 2.88 8.89 13 9 -9 -9.82 9.87 13 -9 -9 -8.14 8.32 13 -9 -8 11.76 7.96 13 9 -8 15.36 8.92 13 9 -8 -3.68 9.49 13 -9 -8 6.64 8.57 13 -9 -8 7.72 8.18 -13 9 8 6.44 4.44 13 -9 -7 -2.11 7.86 13 9 -7 20.79 8.66 13 9 -7 11.49 9.63 13 -9 -7 11.28 8.88 13 -9 -7 -5.72 8.25 -13 9 7 4.33 3.98 13 9 -6 291.14 14.53 13 -9 -6 295.05 14.35 13 -9 -6 270.64 14.53 13 -9 -6 301.49 13.97 13 -9 -5 2.87 7.67 13 9 -5 7.54 8.74 13 -9 -5 -3.26 7.80 13 -9 -5 -3.13 7.94 13 9 -5 -5.53 8.33 13 -9 -4 93.46 10.29 13 9 -4 65.52 10.56 13 -9 -4 100.21 9.63 13 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10.34 13 9 8 185.93 14.24 13 -9 8 174.89 13.61 13 9 8 160.05 13.03 13 -10 -6 41.33 9.55 13 10 -6 28.33 10.20 13 -10 -6 18.35 8.93 13 -10 -6 20.33 8.30 13 10 -6 32.77 8.96 13 -10 -5 0.60 8.42 13 10 -5 -4.36 9.61 13 -10 -5 -18.16 9.09 13 -10 -5 -9.60 8.13 13 10 -5 -9.23 8.90 13 -10 -4 190.48 13.76 13 10 -4 177.68 14.81 13 -10 -4 202.12 13.18 13 -10 -4 196.87 13.00 13 10 -4 194.03 13.35 13 -10 -3 28.12 8.84 13 10 -3 2.76 9.21 13 -10 -3 7.59 8.16 13 10 -3 20.32 8.75 13 -10 -3 5.02 7.89 13 -10 -2 236.89 14.47 13 -10 -2 263.23 14.50 13 -10 -2 233.60 14.10 13 10 -2 228.03 14.64 13 -10 -1 14.84 8.21 13 10 -1 -3.88 8.77 13 -10 -1 3.48 7.53 13 -10 -1 -2.51 7.92 13 10 -1 -1.05 8.50 13 -10 0 79.78 10.07 13 10 0 62.26 9.98 13 -10 0 76.82 9.37 13 -10 0 47.74 8.88 13 10 0 46.98 9.32 13 -10 1 16.40 8.03 13 10 1 16.70 8.72 13 -10 1 15.69 8.03 13 -10 1 12.13 7.77 13 10 1 14.05 8.14 13 10 2 293.68 16.69 13 -10 2 308.43 16.44 13 -10 2 310.31 16.53 13 10 2 305.04 16.68 13 10 3 2.70 7.88 13 -10 3 7.65 8.00 13 -10 3 4.19 7.95 13 10 3 -6.32 8.09 13 10 4 6.57 7.57 13 -10 4 15.48 7.96 13 -10 4 -4.25 8.03 13 10 4 -4.23 8.32 13 10 5 6.59 7.60 13 -10 5 4.32 8.24 13 10 5 0.53 8.27 14 0 -16 347.28 19.71 14 0 -15 7.63 9.18 14 0 -14 125.92 12.06 14 0 -13 7.33 8.84 14 0 -12 286.55 16.85 -14 0 12 286.52 15.98 -14 0 11 3.99 7.46 14 0 -11 -3.90 8.31 -14 0 10 171.04 12.30 14 0 -10 192.83 13.47 14 0 -9 -3.83 8.19 -14 0 9 -2.20 6.91 -14 0 9 1.82 8.22 14 0 -8 125.10 11.60 -14 0 8 152.38 10.88 -14 0 8 135.75 11.81 14 0 -7 2.50 7.75 -14 0 7 3.73 6.82 -14 0 7 8.83 7.60 14 0 -6 357.66 18.71 -14 0 6 378.79 18.40 -14 0 6 343.45 17.46 -14 0 5 5.69 7.28 -14 0 5 -4.16 6.67 14 0 -5 -6.75 7.81 -14 0 4 8.48 7.18 -14 0 4 1.55 6.66 14 0 -4 -8.53 7.64 -14 0 3 6.72 7.93 -14 0 3 1.54 6.22 14 0 -3 5.50 7.34 -14 0 2 232.49 14.25 -14 0 2 254.86 13.88 14 0 -2 235.59 14.62 -14 0 1 -2.04 6.41 14 0 -1 -6.07 7.20 -14 0 0 6.62 6.42 14 0 0 7.29 7.56 -14 0 -1 -7.12 6.74 14 0 1 -0.61 7.52 -14 0 -2 154.89 12.02 -14 0 -2 167.50 11.20 14 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8.49 6.25 15 -5 -8 9.59 8.49 15 5 -8 5.30 8.85 -15 5 7 257.67 13.40 15 -5 -7 248.17 15.84 15 5 -7 280.85 16.68 -15 5 6 -3.76 5.93 15 -5 -6 0.63 8.32 15 5 -6 -5.85 9.21 -15 5 5 13.97 5.81 15 -5 -5 4.39 8.53 15 5 -5 7.08 8.83 -15 5 4 11.32 5.80 15 -5 -4 19.35 8.63 15 5 -4 -2.55 8.51 -15 5 3 366.89 16.09 15 -5 -3 373.76 19.55 15 5 -3 376.44 19.81 -15 5 2 -1.53 4.00 15 -5 -2 -3.12 8.40 15 5 -2 5.06 8.73 15 -5 -1 19.50 8.41 15 5 -1 32.99 9.29 15 -5 0 1.90 8.50 15 5 0 -2.54 8.75 15 -5 1 300.97 16.94 15 5 1 268.93 16.76 -15 -5 -2 1.35 4.49 15 -5 2 -5.74 8.74 15 5 2 -9.55 9.23 -15 -5 -3 52.91 5.87 15 -5 3 62.26 9.91 15 5 3 67.78 10.37 -15 -5 -4 2.07 5.04 15 -5 4 -11.18 8.99 15 5 4 -5.88 8.64 -15 -5 -5 168.49 9.73 15 -5 5 198.29 14.32 15 5 5 172.04 13.56 -15 -5 -6 22.01 5.96 15 -5 6 11.59 9.18 15 5 6 -2.70 8.76 -15 -5 -7 181.88 10.88 15 -5 7 217.26 15.28 15 5 7 217.58 15.16 -15 -5 -8 13.96 6.37 -15 -5 -9 43.99 7.44 15 5 9 34.03 9.14 -15 6 9 143.40 9.96 15 -6 -9 156.56 13.08 15 6 -9 147.43 13.36 15 -6 -8 -5.05 8.98 15 6 -8 4.59 9.34 -15 6 8 6.91 6.01 15 -6 -7 35.73 9.74 15 6 -7 21.46 9.96 -15 6 7 33.16 6.47 15 -6 -6 46.79 9.62 15 6 -6 45.13 9.76 -15 6 6 33.47 6.28 15 -6 -5 216.57 14.49 15 6 -5 242.78 15.24 -15 6 5 197.00 10.77 15 -6 -4 43.92 9.40 15 6 -4 38.00 9.58 15 -6 -3 -1.23 8.79 15 6 -3 -3.77 8.85 -15 6 3 -2.25 4.95 15 -6 -2 3.08 8.70 15 6 -2 10.61 8.49 15 -6 -1 242.66 15.42 15 6 -1 253.95 15.73 15 -6 0 35.71 9.44 15 6 0 28.26 9.00 15 -6 1 29.06 9.65 15 6 1 3.78 9.00 15 -6 2 -4.44 8.88 15 6 2 20.83 9.25 15 6 3 221.38 15.16 15 -6 3 217.05 15.00 15 -6 4 63.89 10.68 15 6 4 38.01 9.97 15 -6 5 88.93 11.19 15 6 5 77.88 10.99 15 -6 6 -1.35 9.80 15 6 6 -8.66 9.20 15 -6 7 99.38 11.87 15 6 7 78.10 11.34 15 -6 8 16.86 10.13 15 6 8 20.73 10.00 15 -7 -6 27.76 5.75 15 -7 -6 21.55 9.11 15 7 -6 33.18 9.87 15 -7 -6 36.30 8.82 15 -7 -5 1.84 8.95 15 7 -5 -1.27 9.27 15 -7 -4 72.15 10.53 15 7 -4 80.94 10.80 15 -7 -3 136.15 12.11 15 7 -3 122.52 12.17 15 -7 -2 94.50 11.29 15 7 -2 117.33 11.77 15 -7 -1 -10.39 9.00 15 7 -1 -8.62 9.10 15 -7 0 14.87 8.89 15 7 0 18.60 9.14 15 -7 1 111.72 11.79 15 7 1 101.39 11.74 15 -7 2 141.22 12.83 15 7 2 161.09 12.99 15 -7 3 21.57 9.19 15 7 3 9.40 9.03 15 -7 4 -9.67 9.73 15 7 4 -9.51 9.76 15 -7 5 74.09 11.25 15 7 5 59.80 10.43 16 0 -10 50.27 10.95 16 0 -9 -7.84 9.46 -16 0 8 186.30 13.39 16 0 -8 180.38 14.09 -16 0 7 -4.20 7.93 16 0 -7 0.70 8.80 -16 0 6 -2.96 8.31 16 0 -6 -1.39 8.87 -16 0 5 15.25 8.34 16 0 -5 0.69 8.54 -16 0 4 315.82 16.98 16 0 -4 304.50 17.97 -16 0 3 -1.74 7.85 16 0 -3 -11.60 9.30 -16 0 2 18.49 8.10 16 0 -2 10.29 8.91 -16 0 1 -2.87 7.92 16 0 -1 0.69 8.80 -16 0 0 198.15 12.98 16 0 0 150.49 13.53 -16 0 -1 -2.26 7.56 16 0 1 -15.09 9.01 -16 0 -2 35.72 8.35 16 0 2 33.80 9.45 16 0 3 8.37 9.01 16 0 4 173.89 13.82 16 0 5 -0.72 8.94 16 0 6 154.12 13.40 16 0 7 -7.37 9.42 -16 0 -8 48.54 10.29 -16 0 -9 -0.58 9.16 -16 1 10 90.84 10.79 16 -1 -10 102.80 12.10 -16 1 9 -1.74 8.07 16 -1 -9 -4.25 9.11 -16 1 8 49.02 8.96 16 -1 -8 45.73 10.36 -16 1 7 42.87 9.03 -16 -1 7 46.40 9.53 16 -1 -7 29.33 9.98 -16 1 6 207.60 13.47 -16 -1 6 205.42 13.93 16 -1 -6 195.57 14.90 -16 1 5 37.39 8.53 -16 -1 5 32.38 9.04 16 -1 -5 26.14 9.42 -16 -1 4 6.19 8.00 -16 1 4 -1.09 7.36 16 -1 -4 -17.08 9.73 -16 -1 3 6.80 8.34 -16 1 3 8.11 7.70 16 -1 -3 15.65 9.55 -16 -1 2 341.60 18.03 -16 1 2 327.39 16.90 16 -1 -2 295.05 18.31 -16 -1 1 42.89 9.17 -16 1 1 49.43 8.47 16 -1 -1 34.88 9.73 -16 1 0 21.08 7.71 -16 -1 0 15.26 7.92 16 -1 0 2.74 9.12 -16 1 -1 3.63 7.11 -16 -1 -1 4.26 8.42 16 -1 1 -7.54 9.19 -16 -1 -2 172.88 12.77 16 -1 2 147.53 13.18 16 -1 3 52.22 10.28 16 -1 4 131.17 12.97 16 -1 5 8.58 9.36 16 -1 6 114.82 12.33 -16 -1 -6 65.53 9.25 16 -1 7 -0.74 9.48 -16 -1 -7 2.87 8.08 -16 -1 -8 93.44 10.60 -16 -1 -9 -2.13 9.10 -16 2 10 121.05 11.37 16 -2 -10 111.66 12.77 16 2 -10 140.23 13.18 -16 2 9 82.40 9.72 16 -2 -9 82.24 11.81 16 2 -9 99.26 12.14 -16 2 8 113.51 10.77 16 -2 -8 123.47 12.63 16 2 -8 119.09 12.56 -16 2 7 6.87 7.76 16 -2 -7 10.40 9.52 16 2 -7 14.76 9.27 -16 2 6 20.80 7.65 16 -2 -6 40.60 10.02 16 2 -6 53.00 10.66 -16 2 5 118.15 10.42 16 -2 -5 107.38 12.07 16 2 -5 107.20 11.94 -16 -2 4 259.67 15.93 -16 2 4 245.65 14.27 16 -2 -4 259.48 16.57 16 2 -4 242.22 16.37 -16 -2 3 102.18 11.06 -16 2 3 102.45 10.02 16 -2 -3 81.14 11.19 16 2 -3 110.59 12.18 -16 -2 2 10.45 8.73 -16 2 2 -3.44 7.16 16 -2 -2 -0.68 8.93 16 2 -2 -2.74 9.24 -16 2 1 31.05 7.83 -16 -2 1 22.12 8.94 16 -2 -1 3.41 9.00 16 2 -1 20.56 9.72 -16 -2 0 130.54 12.48 -16 2 0 183.20 11.67 16 -2 0 163.40 13.60 16 2 0 161.91 13.78 -16 -2 -1 110.28 11.43 16 -2 1 102.50 11.62 16 2 1 108.89 12.10 -16 -2 -2 31.55 9.22 16 -2 2 27.53 9.53 16 2 2 15.16 9.54 16 -2 3 -9.04 9.64 16 2 3 4.87 9.56 16 -2 4 96.52 12.16 16 2 4 129.52 13.09 16 -2 5 122.83 12.61 16 2 5 128.50 12.74 -16 -2 -5 89.57 8.85 16 -2 6 115.97 12.59 -16 -2 -6 93.09 9.68 16 -2 7 10.30 9.79 16 2 7 -13.94 10.40 -16 -2 -7 -4.84 8.19 -16 -2 -8 36.37 8.99 16 -3 -9 -4.17 9.38 16 3 -9 -1.42 9.88 -16 3 9 4.60 7.32 16 -3 -8 53.86 10.69 16 3 -8 45.18 10.59 -16 3 8 48.02 8.18 16 -3 -7 261.50 16.76 16 3 -7 280.84 17.30 -16 3 7 240.00 14.34 16 -3 -6 78.45 11.03 16 3 -6 73.59 11.47 -16 3 6 75.55 8.99 16 -3 -5 111.88 11.85 16 3 -5 88.92 11.82 -16 3 5 75.85 8.77 16 -3 -4 -3.37 9.38 16 3 -4 -5.46 9.61 -16 3 4 -1.85 6.85 16 -3 -3 103.91 11.96 16 3 -3 119.36 12.49 -16 3 3 117.31 9.76 16 -3 -2 119.33 12.55 16 3 -2 138.05 12.88 -16 3 2 132.35 10.18 16 -3 -1 166.06 13.93 16 3 -1 163.68 14.21 16 -3 0 -12.92 9.56 16 3 0 -4.78 9.47 -16 3 0 11.33 6.44 16 -3 1 -0.68 9.43 16 3 1 -7.51 9.50 16 -3 2 42.34 9.89 16 3 2 45.82 10.45 16 -3 3 248.17 16.52 16 3 3 252.15 16.65 16 -3 4 41.29 10.11 16 3 4 37.08 10.30 16 -3 5 -7.83 9.45 16 3 5 -3.55 9.65 16 -3 6 62.13 10.84 16 3 6 51.82 10.82 16 -3 7 152.14 13.82 16 3 7 124.38 13.49 16 -4 -8 4.10 9.41 16 4 -8 -4.91 9.63 -16 4 8 3.71 6.82 16 -4 -7 12.89 9.47 16 4 -7 33.39 10.26 -16 4 7 6.80 6.95 16 -4 -6 -0.68 9.42 16 4 -6 -4.83 9.25 -16 4 6 7.46 6.79 16 -4 -5 265.39 16.55 16 4 -5 251.29 16.75 -16 4 5 246.81 13.46 16 -4 -4 17.39 9.35 16 4 -4 6.11 9.20 -16 4 4 23.67 7.07 16 -4 -3 177.09 14.06 16 4 -3 184.67 14.21 -16 4 3 167.66 10.91 16 -4 -2 4.67 9.09 16 4 -2 -2.69 9.05 -16 4 2 9.68 6.24 16 -4 -1 49.81 10.27 16 4 -1 42.00 10.33 -16 4 1 45.06 6.97 16 -4 0 -12.14 9.71 16 4 0 4.06 9.26 16 -4 1 220.38 15.72 16 4 1 253.91 16.16 16 -4 2 7.49 9.30 16 4 2 -9.52 9.57 16 -4 3 -6.89 9.80 16 4 3 -2.06 9.19 16 -4 4 4.19 9.32 16 4 4 -0.69 9.61 16 -4 5 288.53 18.38 16 4 5 327.88 18.57 16 -4 6 4.32 9.77 16 4 6 17.16 10.15 16 -5 -6 -4.01 9.82 16 5 -6 -4.10 9.64 -16 5 6 3.13 6.23 16 -5 -5 86.45 11.30 16 5 -5 75.34 11.07 -16 5 5 85.99 8.21 16 -5 -4 3.98 9.34 16 5 -4 4.72 9.37 -16 5 4 -2.50 6.03 16 -5 -3 105.00 11.82 16 5 -3 101.72 12.18 -16 5 3 110.12 8.42 16 -5 -2 -7.92 8.90 16 5 -2 -12.65 9.78 -16 5 2 5.33 5.52 16 -5 -1 135.50 12.99 16 5 -1 145.33 13.32 16 -5 0 -9.38 9.67 16 5 0 -6.04 9.64 16 -5 1 54.63 10.43 16 5 1 28.96 10.06 16 -5 2 14.23 9.76 16 5 2 6.75 9.75 16 -5 3 351.97 19.75 16 5 3 331.99 19.14 16 -5 4 -6.93 9.92 16 5 4 -2.75 9.40 17 0 -4 72.21 11.49 -17 0 4 72.97 10.46 17 0 -3 -12.20 9.71 -17 0 3 -6.10 8.50 17 0 -2 188.32 15.11 -17 0 2 189.08 13.56 17 0 -1 2.17 9.56 -17 0 1 -1.20 8.37 17 0 0 26.78 10.02 -17 0 0 27.94 8.87 17 0 1 -13.04 10.35 -17 0 -1 -4.10 8.29 17 0 2 126.22 13.06 17 -1 -4 102.87 12.04 -17 1 4 119.30 11.25 17 -1 -3 -5.01 9.76 -17 1 3 2.84 7.99 17 -1 -2 20.08 9.88 -17 1 2 27.52 8.63 -17 -1 2 35.41 9.59 17 -1 -1 27.39 9.51 -17 -1 1 35.87 9.49 -17 1 1 36.68 8.95 17 -1 0 89.44 11.98 -17 -1 0 95.02 10.97 -17 1 0 85.30 10.16 17 -1 1 10.13 9.88 -17 -1 -1 2.53 8.77 17 -1 2 31.89 10.27 17 -2 -2 111.88 12.46 17 2 -2 96.75 12.31 -17 2 2 98.78 10.34 17 -2 -1 -12.91 10.63 17 2 -1 -19.47 11.02 -17 2 1 -2.02 7.49 17 -2 0 24.47 10.36 17 2 0 36.07 11.09 -17 2 0 33.50 8.01 0 0 0 0.00 0.00 TITL Rah20_abs in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 13.386461 12.681121 21.586230 90.0000 91.7234 90.0000 ZERR 4.00 0.000300 0.000192 0.000403 0.0000 0.0019 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C B N O F Bi UNIT 136.00 160.00 24.00 40.00 12.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 67534 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.555 _oxdiff_exptl_absorpt_empirical_full_min 0.746