#------------------------------------------------------------------------------ #$Date: 2024-10-06 03:20:07 +0300 (Sun, 06 Oct 2024) $ #$Revision: 295078 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249429.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7249429 loop_ _publ_author_name 'Valdivieso, Jorge P.' 'Erickson, Alexander N.' 'Gardinier, James R.' _publ_section_title ; Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand ; _journal_issue 43 _journal_name_full 'RSC Advances' _journal_page_first 31502 _journal_page_last 31516 _journal_paper_doi 10.1039/D4RA05287K _journal_volume 14 _journal_year 2024 _chemical_formula_moiety 'C30 H25 Br N4 O3 P Re' _chemical_formula_sum 'C30 H25 Br N4 O3 P Re' _chemical_formula_weight 786.62 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-03-20 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-07-17 deposited with the CCDC. 2024-09-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.9290(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.3314(2) _cell_length_b 13.5371(2) _cell_length_c 17.3610(3) _cell_measurement_reflns_used 12870 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 70.6110 _cell_measurement_theta_min 3.6430 _cell_volume 2824.62(8) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3756 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _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 -117.00 -18.00 1.00 1.00 -- -42.46 -37.00 30.00 99 2 \w -81.00 27.00 1.00 1.00 -- -42.46 93.00 -67.00 108 3 \w 23.00 98.00 1.00 1.00 -- 42.46-125.00-150.00 75 4 \w 101.00 178.00 1.00 1.12 -- 100.00 93.00 -67.00 77 5 \w 27.00 118.00 1.00 1.12 -- 100.00-125.00 120.00 91 6 \w 27.00 118.00 1.00 1.12 -- 100.00-125.00 30.00 91 7 \w 27.00 118.00 1.00 1.12 -- 100.00-125.00-120.00 91 8 \w 74.00 173.00 1.00 1.12 -- 100.00 45.00 0.00 99 9 \w 47.00 178.00 1.00 1.12 -- 100.00 15.00 120.00 131 10 \w 94.00 173.00 1.00 1.12 -- 100.00 125.00 150.00 79 11 \w -119.00 -10.00 1.00 1.00 -- -42.46 -77.00 -30.00 109 12 \w -115.00 -14.00 1.00 1.00 -- -42.46 -57.00-120.00 101 13 \w -115.00 -14.00 1.00 1.00 -- -42.46 -57.00 150.00 101 14 \w 94.00 140.00 1.00 1.12 -- 100.00 125.00 30.00 46 15 \w 71.00 172.00 1.00 1.12 -- 100.00 61.00-180.00 101 16 \w 72.00 176.00 1.00 1.12 -- 100.00 30.00 -90.00 104 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0817770000 _diffrn_orient_matrix_UB_12 -0.0761836000 _diffrn_orient_matrix_UB_13 -0.0468062000 _diffrn_orient_matrix_UB_21 -0.0290889000 _diffrn_orient_matrix_UB_22 0.0724356000 _diffrn_orient_matrix_UB_23 -0.0700478000 _diffrn_orient_matrix_UB_31 0.0942451000 _diffrn_orient_matrix_UB_32 -0.0436512000 _diffrn_orient_matrix_UB_33 -0.0345635000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 26425 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 70.648 _diffrn_reflns_theta_max 70.648 _diffrn_reflns_theta_min 4.007 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 10.932 _exptl_absorpt_correction_T_max 0.636 _exptl_absorpt_correction_T_min 0.135 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 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_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.850 _exptl_crystal_description prism _exptl_crystal_F_000 1528 _exptl_crystal_size_max 0.321 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.967 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 5354 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.138 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0302 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+4.0831P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.0737 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4982 _reflns_number_total 5354 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra05287k3.cif _cod_data_source_block 1_gard25y _cod_database_code 7249429 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula C30H25BrN4O3PRe _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. ; _shelx_estimated_absorpt_t_max 0.354 _shelx_estimated_absorpt_t_min 0.127 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: Br1A(0.8) Br1B(0.2) O2A(0.8) O2B(0.2) C9A(0.8) C9B(0.2) 3.a Ternary CH refined with riding coordinates: C7(H7) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21), C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45), C46(H46) 3.c Idealised Me refined as rotating group: C37(H37A,H37B,H37C), C47(H47A,H47B,H47C) ; _shelx_res_file ; TITL gard25y_a.res in P2(1)/n gard25y.res created by SHELXL-2018/1 at 15:52:21 on 20-Mar-2024 REM Old TITL GARD25Y in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.079, Rweak 0.014, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C30 N3 O3 P Br Re CELL 1.54184 12.3314 13.5371 17.361 90 102.929 90 ZERR 4 0.0002 0.0002 0.0003 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O P Br Re UNIT 120 100 16 12 4 4 4 L.S. 7 PLAN 6 SIZE 0.12 0.2 0.321 TEMP 100 CONF BOND $H list 4 MORE -1 fmap 2 acta 144 REM REM REM WGHT 0.034000 4.083100 FVAR 0.23249 RE1 7 0.598426 0.472834 0.346693 11.00000 0.01528 0.01709 = 0.01986 0.00284 0.00306 -0.00133 PART 1 BR1A 6 0.496529 0.634295 0.371725 10.80000 0.02138 0.01614 = 0.02304 -0.00162 0.00659 -0.00118 PART -1 BR1B 6 0.677226 0.300226 0.346517 10.20000 0.02623 0.02888 = 0.02926 0.00639 0.00910 0.00285 PART 0 P1 5 0.541166 0.489648 0.200428 11.00000 0.01530 0.01363 = 0.01985 -0.00098 0.00472 -0.00101 O3 4 0.694299 0.463671 0.527562 11.00000 0.04158 0.03589 = 0.02294 0.00376 -0.00026 -0.00599 O1 4 0.816436 0.575480 0.335821 11.00000 0.02072 0.04855 = 0.04301 0.00905 0.00628 -0.01161 PART 1 O2A 4 0.696316 0.265040 0.336502 10.80000 0.03752 0.02996 = 0.04373 0.00794 0.01561 0.01486 PART -1 O2B 4 0.481496 0.665713 0.373272 10.20000 0.01762 PART 0 N11 3 0.337224 0.410305 0.318193 11.00000 0.01597 0.01901 = 0.02275 -0.00153 0.00609 -0.00107 N12 3 0.444769 0.396170 0.358389 11.00000 0.01739 0.01609 = 0.02019 -0.00019 0.00560 -0.00212 N21 3 0.209280 0.524635 0.241362 11.00000 0.01668 0.01900 = 0.02344 -0.00195 0.00308 0.00204 N22 3 0.108441 0.477949 0.226158 11.00000 0.01504 0.02976 = 0.04553 -0.00797 0.00562 0.00085 C1 1 0.423952 0.411912 0.150120 11.00000 0.01955 0.01582 = 0.01974 0.00001 0.00381 0.00031 C2 1 0.323093 0.410599 0.175657 11.00000 0.01602 0.01443 = 0.02023 0.00271 0.00411 -0.00013 C3 1 0.238049 0.347829 0.138983 11.00000 0.01714 0.01807 = 0.02629 0.00085 0.00462 0.00063 AFIX 43 H3 2 0.171756 0.346468 0.156056 11.00000 -1.20000 AFIX 0 C4 1 0.250675 0.287211 0.077297 11.00000 0.02193 0.01976 = 0.03149 -0.00391 0.00375 -0.00611 AFIX 43 H4 2 0.193161 0.245241 0.053553 11.00000 -1.20000 AFIX 0 C5 1 0.348675 0.288869 0.050834 11.00000 0.02874 0.02391 = 0.02381 -0.00617 0.00789 -0.00182 AFIX 43 H5 2 0.357060 0.248342 0.009303 11.00000 -1.20000 AFIX 0 C6 1 0.434281 0.351539 0.086829 11.00000 0.02155 0.01931 = 0.02511 -0.00094 0.00807 0.00009 AFIX 43 H6 2 0.499585 0.353366 0.068508 11.00000 -1.20000 AFIX 0 C7 1 0.312848 0.472513 0.246461 11.00000 0.01591 0.01325 = 0.02521 0.00160 0.00615 -0.00060 AFIX 13 H7 2 0.371525 0.522678 0.253276 11.00000 -1.20000 AFIX 0 C10 1 0.654734 0.466618 0.462456 11.00000 0.02314 0.01974 = 0.02615 0.00280 0.00450 -0.00194 C8 1 0.734429 0.538025 0.339335 11.00000 0.02290 0.02692 = 0.02103 0.00254 0.00021 -0.00096 PART 1 C9A 1 0.660415 0.345846 0.336076 10.80000 0.02506 0.02267 = 0.02896 0.00965 0.00493 -0.00474 PART -1 C9B 1 0.527003 0.600720 0.368437 10.20000 0.02455 PART 0 C11 1 0.267722 0.349595 0.344592 11.00000 0.01895 0.02662 = 0.03226 0.00096 0.00975 -0.00456 AFIX 43 H11 2 0.191277 0.344669 0.325086 11.00000 -1.20000 AFIX 0 C12 1 0.330584 0.295861 0.405985 11.00000 0.02722 0.03165 = 0.03205 0.00660 0.01013 -0.00456 AFIX 43 H12 2 0.305632 0.248695 0.436928 11.00000 -1.20000 AFIX 0 C13 1 0.438563 0.327114 0.411669 11.00000 0.02646 0.02577 = 0.02616 0.00584 0.00641 -0.00273 AFIX 43 H13 2 0.499588 0.302829 0.448316 11.00000 -1.20000 AFIX 0 C21 1 0.199884 0.621052 0.259049 11.00000 0.02642 0.02087 = 0.04678 -0.00325 0.00656 0.00315 AFIX 43 H21 2 0.257622 0.666534 0.271986 11.00000 -1.20000 AFIX 0 C22 1 0.090174 0.639001 0.254364 11.00000 0.02890 0.02733 = 0.05763 -0.01255 0.00445 0.00881 AFIX 43 H22 2 0.057411 0.698652 0.263003 11.00000 -1.20000 AFIX 0 C23 1 0.037672 0.549173 0.233926 11.00000 0.01929 0.03561 = 0.03604 -0.00447 0.00598 0.00588 AFIX 43 H23 2 -0.038689 0.539832 0.226478 11.00000 -1.20000 AFIX 0 C31 1 0.654469 0.460419 0.151149 11.00000 0.01440 0.01735 = 0.02364 0.00060 0.00457 -0.00002 C32 1 0.697897 0.531630 0.108666 11.00000 0.02070 0.01798 = 0.02966 0.00285 0.00602 0.00204 AFIX 43 H32 2 0.666721 0.594504 0.103214 11.00000 -1.20000 AFIX 0 C33 1 0.785968 0.511129 0.074518 11.00000 0.01886 0.01972 = 0.03174 0.00380 0.00773 -0.00217 AFIX 43 H33 2 0.813072 0.560167 0.046338 11.00000 -1.20000 AFIX 0 C34 1 0.835280 0.417339 0.081680 11.00000 0.01683 0.02215 = 0.01867 -0.00070 0.00160 -0.00052 C35 1 0.791786 0.346583 0.124122 11.00000 0.02297 0.01915 = 0.02181 0.00170 0.00652 0.00257 AFIX 43 H35 2 0.822770 0.283632 0.129362 11.00000 -1.20000 AFIX 0 C36 1 0.703940 0.366873 0.158771 11.00000 0.02472 0.01669 = 0.02552 0.00358 0.00870 0.00246 AFIX 43 H36 2 0.677396 0.318004 0.187415 11.00000 -1.20000 AFIX 0 C37 1 0.932033 0.396953 0.045039 11.00000 0.02569 0.02164 = 0.02903 0.00261 0.01161 0.00185 AFIX 137 H37A 2 0.994418 0.436446 0.070580 11.00000 -1.50000 H37B 2 0.912221 0.413064 -0.010184 11.00000 -1.50000 H37C 2 0.951467 0.328283 0.051239 11.00000 -1.50000 AFIX 0 C41 1 0.501877 0.613425 0.161697 11.00000 0.01741 0.01554 = 0.02235 0.00086 0.01005 0.00154 C42 1 0.427776 0.627569 0.089502 11.00000 0.01924 0.01778 = 0.02187 -0.00040 0.00573 -0.00011 AFIX 43 H42 2 0.388004 0.574285 0.063553 11.00000 -1.20000 AFIX 0 C43 1 0.413050 0.720860 0.056131 11.00000 0.02113 0.02372 = 0.01968 0.00364 0.00614 0.00450 AFIX 43 H43 2 0.363426 0.729240 0.007665 11.00000 -1.20000 AFIX 0 C44 1 0.470984 0.802762 0.093540 11.00000 0.02301 0.01959 = 0.02596 0.00097 0.01305 0.00220 C45 1 0.542953 0.787824 0.166611 11.00000 0.02173 0.01583 = 0.02844 -0.00139 0.00642 -0.00184 AFIX 43 H45 2 0.581055 0.841416 0.193345 11.00000 -1.20000 AFIX 0 C46 1 0.558969 0.695145 0.200237 11.00000 0.01972 0.01985 = 0.02210 0.00296 0.00416 0.00003 AFIX 43 H46 2 0.608120 0.686922 0.248922 11.00000 -1.20000 AFIX 0 C47 1 0.457815 0.903459 0.056293 11.00000 0.03113 0.02710 = 0.03547 0.01118 0.00606 0.00296 AFIX 137 H47A 2 0.409620 0.942747 0.080351 11.00000 -1.50000 H47B 2 0.426119 0.897226 0.000733 11.00000 -1.50000 H47C 2 0.529288 0.934768 0.063988 11.00000 -1.50000 AFIX 0 HKLF 4 REM gard25y_a.res in P2(1)/n REM R1 = 0.0302 for 4982 Fo > 4sig(Fo) and 0.0337 for all 5354 data REM 380 parameters refined using 0 restraints END WGHT 0.0340 4.0830 REM Highest difference peak 0.967, deepest hole -1.069, 1-sigma level 0.117 Q1 1 0.6353 0.4782 0.4131 11.00000 0.05 0.97 Q2 1 0.5237 0.4738 0.3362 11.00000 0.05 0.93 Q3 1 0.5728 0.4626 0.2915 11.00000 0.05 0.83 Q4 1 0.6732 0.4721 0.3598 11.00000 0.05 0.78 Q5 1 0.6949 0.2223 0.2653 11.00000 0.05 0.44 Q6 1 0.6182 0.5408 0.2919 11.00000 0.05 0.43 ; _shelx_res_checksum 64592 _shelx_hkl_file ; 0 0 -2 2600.16 24.58 0 0 2 2585.51 21.30 0 0 -3 1.03 1.61 0 0 3 1.91 1.69 0 0 -4 7674.83 61.83 0 0 4 7572.01 52.71 0 0 5 4.46 3.19 0 0 -5 6.83 3.19 0 0 -6 2651.78 47.04 0 0 6 2571.33 37.97 0 0 -7 1.51 3.96 0 0 7 5.07 4.85 0 0 8 102.20 10.30 0 0 -8 122.05 12.85 0 0 -9 5.47 3.44 0 0 9 4.55 6.32 0 0 10 4141.58 67.74 0 0 -10 4130.90 82.62 0 0 -11 11.01 4.15 0 0 11 2.81 5.73 0 0 -11 14.03 6.01 0 0 12 510.06 28.47 0 0 -12 600.76 30.08 0 0 -12 597.72 27.52 0 0 -12 624.02 38.18 0 0 12 582.55 29.67 0 0 13 3.47 3.69 0 0 -13 18.13 4.80 0 0 -13 -1.11 4.69 0 0 13 1.92 8.28 0 0 14 476.11 30.77 0 0 -14 497.94 26.59 0 0 -14 474.21 30.39 0 0 14 450.96 29.75 0 0 -15 8.69 7.20 0 0 15 7.93 6.87 0 0 -15 1.56 9.70 0 0 16 593.96 33.74 0 0 -16 638.67 40.04 0 0 -16 656.84 35.45 0 0 17 -11.05 6.84 0 0 -17 6.87 4.75 0 0 -17 5.10 9.19 0 0 18 43.93 8.47 0 0 -18 41.68 12.86 0 0 -18 47.91 10.65 0 0 -19 -0.27 5.32 0 0 19 3.42 3.43 0 0 20 379.38 19.93 0 0 -20 364.77 18.14 0 -1 1 1179.34 13.90 0 1 -1 1306.66 17.07 0 1 1 1409.77 15.18 0 -1 1 1231.66 12.38 0 1 -2 66.35 4.17 0 1 -2 66.84 3.79 0 -1 -2 50.35 2.70 0 -1 -2 49.57 2.57 0 -1 2 56.45 3.55 0 1 2 68.01 4.06 0 -1 2 67.69 2.88 0 -1 -2 62.79 5.53 0 -1 -3 2625.31 20.20 0 1 -3 2562.46 28.31 0 -1 -3 2583.01 17.06 0 -1 3 2551.78 16.18 0 1 3 2503.96 26.91 0 1 -3 2661.23 28.13 0 -1 -3 2655.92 37.85 0 -1 3 2518.92 26.43 0 -1 4 203.15 9.16 0 1 -4 205.54 9.85 0 -1 -4 223.38 6.26 0 -1 -4 225.34 4.69 0 -1 4 213.00 4.36 0 -1 -4 228.62 12.71 0 1 4 210.20 9.54 0 1 -5 2.35 2.46 0 -1 -5 3.26 3.81 0 -1 -5 0.44 0.43 0 -1 5 4.30 2.72 0 1 5 4.42 3.32 0 1 -6 113.90 9.61 0 1 6 118.78 9.26 0 -1 6 117.51 9.00 0 -1 -6 106.65 4.82 0 -1 -6 107.61 10.80 0 1 7 5746.63 63.54 0 1 -7 5642.49 71.33 0 -1 -7 5546.49 76.01 0 -1 7 5449.15 61.07 0 -1 8 24.38 6.04 0 1 -8 44.06 8.31 0 1 8 38.56 7.59 0 -1 -8 43.35 8.43 0 -1 -9 1391.96 45.48 0 1 -9 1467.03 45.78 0 -1 9 1376.46 36.56 0 1 9 1400.02 37.11 0 1 10 438.26 23.51 0 -1 -10 479.66 28.87 0 -1 10 440.24 23.54 0 1 -10 467.88 27.90 0 -1 11 507.24 25.93 0 1 11 513.51 26.67 0 -1 11 494.73 26.21 0 -1 -11 519.69 25.79 0 -1 -11 574.68 29.62 0 1 -11 557.38 33.33 0 1 -12 1.23 7.08 0 -1 12 9.89 7.01 0 1 12 3.34 4.96 0 -1 12 -0.86 6.49 0 -1 -12 9.05 5.93 0 1 -12 9.80 4.83 0 -1 -12 14.69 7.24 0 -1 -13 805.33 37.88 0 -1 -13 772.22 33.88 0 1 13 718.64 35.69 0 1 -13 870.93 45.71 0 1 13 708.99 34.99 0 -1 13 709.71 35.21 0 1 -13 786.78 36.13 0 -1 13 730.02 34.73 0 1 14 288.57 23.70 0 1 -14 326.83 24.42 0 -1 -14 320.91 25.11 0 -1 -14 291.44 27.02 0 -1 14 320.68 26.70 0 1 14 216.57 21.30 0 -1 -14 308.24 22.64 0 -1 14 293.15 22.99 0 -1 15 76.28 13.26 0 -1 -15 98.12 13.72 0 1 15 61.94 12.74 0 1 -15 88.56 14.07 0 -1 -15 88.85 15.65 0 -1 -15 90.77 16.60 0 1 -16 17.67 5.96 0 -1 -16 13.64 8.92 0 -1 16 9.33 5.73 0 1 -16 3.74 10.04 0 -1 -16 1.87 9.51 0 1 16 4.28 8.10 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6.79 4 -12 -14 49.87 6.36 -4 -12 13 47.58 7.53 4 12 -13 35.25 7.47 4 -12 -13 43.06 7.27 4 -12 -12 33.72 6.39 -4 -12 12 28.37 7.64 4 12 -12 42.83 9.96 -4 -12 11 323.30 22.48 4 12 -11 303.28 23.32 4 -12 -11 281.43 21.14 -4 -12 10 133.23 15.74 4 -12 -10 95.83 14.56 4 12 -10 144.29 17.13 -4 -12 9 760.93 37.67 4 12 -9 786.94 40.40 4 -12 -9 687.17 36.40 4 -12 -8 53.79 13.30 -4 -12 8 50.83 12.32 4 12 -8 48.43 14.28 -4 12 8 46.67 9.33 4 12 -8 40.57 8.75 4 12 -7 -0.24 5.94 4 -12 -7 14.57 9.55 -4 -12 7 -0.49 8.50 4 12 -7 -0.68 9.26 4 12 -6 33.40 8.43 4 -12 -6 20.31 9.60 -4 -12 6 27.92 11.69 4 12 -6 8.12 7.94 -4 -12 5 235.13 24.39 4 12 -5 210.13 21.76 4 12 -5 228.28 20.31 4 -12 -5 210.99 22.23 4 -12 -4 7.21 7.74 -4 -12 4 4.32 10.66 4 12 -4 5.64 4.11 4 12 -3 174.50 16.26 4 12 -3 161.11 18.78 4 -12 -3 143.83 17.00 -4 -12 3 196.42 21.93 -4 -12 2 72.26 17.38 4 12 -2 54.88 11.78 4 12 -2 75.92 10.55 4 -12 -2 79.72 13.92 -4 -12 1 45.03 14.87 4 12 -1 49.04 8.93 4 12 -1 52.38 9.91 -4 -12 0 15.00 9.11 4 12 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2 -7 12.48 10.38 10 -2 -6 584.06 34.65 10 -2 -6 582.53 34.64 10 2 -6 485.69 34.03 10 -2 -6 603.00 36.09 -10 -2 6 431.50 31.77 10 -2 -6 558.56 33.75 10 2 -6 534.97 34.64 10 2 -6 507.90 31.35 10 -2 -6 551.38 31.07 10 -2 -5 85.45 15.32 10 -2 -5 99.62 17.49 10 2 -5 95.95 14.81 10 -2 -5 95.13 13.67 -10 -2 5 102.90 18.50 10 -2 -5 74.08 13.43 10 2 -5 89.46 13.38 -10 2 5 90.39 15.44 10 2 -5 79.39 12.19 10 -2 -5 97.54 13.22 10 -2 -4 573.29 34.03 10 -2 -4 580.23 34.52 10 2 -4 560.52 36.09 10 -2 -4 575.16 34.87 -10 -2 4 602.32 38.68 10 -2 -4 570.05 34.06 10 2 -4 525.41 33.13 10 2 -4 527.21 31.34 10 -2 -4 582.29 30.96 10 -2 -3 30.77 9.96 10 -2 -3 31.15 11.76 10 2 -3 22.92 7.45 -10 2 3 24.73 10.74 -10 -2 3 16.49 8.14 10 -2 -3 31.57 9.54 10 2 -3 22.50 8.02 10 -2 -3 12.69 7.69 10 2 -3 8.65 7.15 10 -2 -3 32.19 8.43 10 -2 -2 57.56 11.63 10 -2 -2 53.59 12.96 10 2 -2 37.18 9.33 -10 2 2 43.83 10.81 -10 -2 2 58.46 12.78 10 -2 -2 49.53 11.20 10 2 -2 42.26 9.17 10 -2 -2 49.34 12.16 10 2 -2 49.40 11.36 10 -2 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6.13 3.39 -10 4 -9 94.45 12.32 10 4 9 91.34 10.91 -10 -4 -9 103.61 11.14 10 4 9 108.42 10.71 -10 4 -10 343.75 20.95 10 4 10 344.06 18.53 -10 -4 -10 348.91 17.81 10 4 10 352.07 16.60 -10 4 -11 168.89 13.62 -10 -4 -11 174.21 10.87 -10 -4 -11 161.30 10.74 -10 -4 -11 183.41 11.54 10 -5 -17 245.95 14.08 10 -5 -16 53.60 8.97 10 -5 -16 56.63 7.06 10 -5 -15 18.78 8.15 10 -5 -15 4.86 2.50 10 -5 -14 44.11 7.08 10 -5 -14 33.32 11.02 10 -5 -13 196.64 18.76 10 -5 -13 202.05 18.28 10 -5 -13 193.69 16.72 10 -5 -12 305.69 25.13 10 -5 -12 339.09 24.90 10 -5 -12 318.26 22.60 10 -5 -11 138.82 17.59 10 -5 -11 105.25 16.86 10 -5 -11 127.72 15.07 10 -5 -10 26.92 10.14 10 -5 -10 14.87 10.08 10 -5 -10 26.28 10.08 10 5 -10 44.38 10.65 10 -5 -9 231.93 23.16 10 -5 -9 228.73 22.36 10 5 -9 248.85 22.81 10 -5 -9 230.84 20.09 10 -5 -8 395.02 30.90 10 -5 -8 387.26 28.54 10 5 -8 367.78 27.95 10 -5 -8 350.01 24.74 10 -5 -7 560.08 37.00 10 -5 -7 532.77 32.48 10 5 -7 531.14 33.47 10 -5 -7 444.99 27.70 10 -5 -6 610.06 38.79 10 -5 -6 607.88 33.99 10 5 -6 571.74 34.21 10 -5 -6 557.36 30.57 10 -5 -5 0.56 6.90 10 -5 -5 7.02 12.59 10 -5 -5 16.05 5.17 10 5 -5 14.35 4.45 10 5 -5 14.75 6.86 10 -5 -4 231.03 26.36 10 -5 -4 226.96 21.51 10 5 -4 216.22 18.39 10 5 -4 196.05 20.58 10 -5 -4 242.49 19.35 10 -5 -3 295.20 24.26 10 5 -3 285.65 21.50 10 5 -3 259.35 22.98 10 -5 -3 305.23 22.20 10 -5 -2 1375.23 49.40 10 5 -2 1269.75 47.13 10 5 -2 1367.90 46.10 -10 -5 1 229.38 22.14 10 -5 -1 229.87 20.47 10 5 -1 197.35 19.34 10 5 -1 190.20 17.73 -10 -5 0 26.33 10.03 10 -5 0 46.60 9.96 10 5 0 34.57 7.21 10 5 0 35.75 9.20 -10 -5 -1 39.31 10.25 10 -5 1 47.00 10.38 10 5 1 33.83 7.19 10 5 1 45.90 9.01 -10 -5 -2 1177.73 44.63 10 -5 2 1219.83 42.76 10 5 2 1194.17 43.16 10 5 2 1100.44 40.47 10 5 3 589.49 28.49 -10 -5 -3 590.42 32.13 10 5 3 554.59 29.08 10 5 3 577.71 29.52 -10 5 -4 366.54 25.32 10 5 4 374.11 23.27 -10 -5 -4 324.38 22.84 10 -5 4 314.37 22.59 10 5 4 380.40 22.74 10 5 4 323.46 22.30 -10 5 -5 322.36 23.56 10 5 5 303.24 21.10 -10 -5 -5 324.41 23.26 10 -5 5 275.49 20.20 10 5 5 276.41 21.40 -10 5 -6 269.15 21.72 10 5 6 276.25 20.34 -10 -5 -6 278.78 20.69 10 -5 6 245.46 18.44 10 5 6 308.26 20.99 -10 5 -7 52.49 10.54 10 5 7 38.66 8.65 -10 -5 -7 45.66 8.06 10 -5 7 46.32 7.64 10 5 7 46.39 8.38 -10 5 -8 401.05 24.85 10 5 8 407.49 22.23 -10 -5 -8 427.43 22.43 10 5 8 446.04 22.05 -10 5 -9 300.91 19.97 10 5 9 284.22 17.34 -10 -5 -9 315.14 17.78 10 5 9 306.17 16.78 -10 5 -10 16.88 5.33 10 5 10 12.60 4.66 -10 -5 -10 22.46 4.77 10 5 10 12.93 3.15 -10 -5 -11 7.45 3.56 10 -6 -16 4.08 3.91 10 -6 -16 10.95 2.94 10 -6 -15 129.56 12.42 10 -6 -15 131.11 10.99 10 -6 -14 37.74 6.43 10 -6 -14 39.49 8.89 10 -6 -13 57.45 10.78 10 -6 -13 56.92 8.63 10 -6 -12 10.56 5.51 10 -6 -12 10.14 8.14 10 -6 -12 5.62 7.40 10 -6 -11 274.70 23.12 10 -6 -11 315.81 24.44 10 -6 -11 270.16 21.88 10 -6 -10 239.37 23.98 10 -6 -10 267.44 22.97 10 6 -10 302.93 22.43 10 -6 -10 240.51 20.93 10 -6 -9 667.52 36.62 10 -6 -9 710.06 36.99 10 -6 -9 736.15 34.51 10 -6 -8 176.21 21.14 10 -6 -8 188.46 19.45 10 6 -8 190.83 19.10 10 -6 -8 182.11 18.67 10 -6 -7 2.39 5.91 10 -6 -7 5.05 11.88 10 -6 -7 14.68 5.84 10 6 -7 -0.56 5.60 10 -6 -6 47.71 10.57 10 -6 -6 35.20 17.29 10 -6 -6 41.66 10.71 10 6 -6 13.05 9.27 10 -6 -5 1372.88 58.36 10 -6 -5 1355.69 49.11 10 6 -5 1276.26 47.95 10 -6 -5 1244.26 43.57 10 -6 -4 464.57 35.82 10 -6 -4 485.01 30.23 10 6 -4 495.74 25.81 10 6 -4 436.27 29.59 10 -6 -4 469.34 26.95 10 -6 -3 136.59 16.07 10 6 -3 131.33 13.30 10 6 -3 122.99 16.42 10 -6 -3 144.10 15.68 10 -6 -2 1.69 6.04 10 6 -2 -1.83 4.77 10 6 -2 -0.60 5.81 -10 -6 1 620.49 34.66 10 -6 -1 640.53 32.47 10 6 -1 595.96 32.73 10 6 -1 608.98 28.94 -10 -6 0 278.03 23.85 10 -6 0 310.94 22.26 10 6 0 252.49 21.39 10 6 0 243.52 18.75 -10 -6 -1 939.22 40.69 10 -6 1 960.49 36.92 10 6 1 873.64 37.69 10 6 1 860.20 34.60 -10 -6 -2 38.44 11.20 10 6 2 28.20 8.35 10 6 2 37.48 8.31 10 6 3 1.76 3.51 -10 -6 -3 15.42 10.07 10 6 3 1.81 6.63 10 6 3 13.67 5.52 10 6 4 39.60 7.10 -10 -6 -4 35.41 9.23 10 -6 4 35.44 7.68 10 6 4 31.49 8.89 10 6 4 46.39 7.85 -10 6 -5 694.58 33.01 10 6 5 737.31 31.06 -10 -6 -5 750.80 33.22 10 -6 5 635.46 31.17 10 6 5 762.05 31.95 -10 6 -6 65.31 9.39 -10 -6 -6 66.16 10.88 10 6 6 51.14 10.17 10 -6 6 40.59 8.93 10 6 6 55.13 10.73 10 6 7 49.28 8.58 -10 6 -7 37.21 8.69 -10 -6 -7 32.07 8.08 10 -6 7 38.39 8.14 10 6 7 48.69 7.90 10 6 8 43.19 7.96 -10 6 -8 29.47 8.23 -10 -6 -8 46.05 7.85 10 6 8 43.76 6.94 -10 6 -9 332.78 19.11 10 6 9 328.38 17.09 -10 -6 -9 341.38 17.61 10 6 9 339.73 16.49 -10 -6 -10 256.35 13.61 10 6 10 252.65 12.54 -10 -6 -10 231.57 12.67 10 -7 -15 33.86 5.20 10 -7 -15 42.38 6.66 10 -7 -14 102.91 10.40 10 -7 -14 96.34 9.92 10 -7 -13 5.12 3.23 10 -7 -13 3.08 5.56 10 -7 -12 415.27 23.64 10 -7 -12 414.50 23.10 10 -7 -11 149.05 16.98 10 -7 -11 158.11 16.88 10 -7 -11 142.62 14.93 10 -7 -10 49.12 10.58 10 -7 -10 49.88 12.41 10 -7 -10 45.24 11.10 10 7 -10 46.80 9.32 10 -7 -9 11.26 7.87 10 -7 -9 25.63 12.15 10 -7 -9 22.15 6.39 10 7 -9 26.08 6.67 10 -7 -8 524.06 32.89 10 -7 -8 586.80 32.68 10 7 -8 573.16 30.80 10 -7 -8 519.54 29.72 10 -7 -7 154.61 20.76 10 -7 -7 115.72 15.20 10 7 -7 156.56 17.56 10 -7 -7 151.62 17.50 10 -7 -6 700.58 40.08 10 -7 -6 776.90 37.03 10 7 -6 727.39 34.91 10 -7 -6 670.56 32.39 10 -7 -5 9.33 5.92 10 -7 -5 27.14 8.99 10 7 -5 6.78 7.63 10 -7 -4 319.60 23.69 10 7 -4 317.75 23.87 10 -7 -4 325.62 21.99 10 -7 -3 142.32 15.50 10 7 -3 141.92 12.92 10 7 -3 123.22 16.45 -10 -7 2 1092.88 45.15 10 -7 -2 1126.80 42.01 10 7 -2 997.71 34.57 10 7 -2 1067.91 42.45 -10 -7 1 164.09 19.41 10 -7 -1 187.56 17.16 10 7 -1 147.53 14.14 10 7 -1 169.22 17.39 -10 -7 0 33.50 11.08 10 -7 0 25.89 6.67 10 7 0 10.74 6.30 10 7 0 35.34 9.39 -10 -7 -1 45.24 10.78 10 7 1 36.72 8.29 10 7 1 44.80 8.21 -10 -7 -2 779.47 35.14 10 7 2 770.23 33.51 10 7 2 719.33 30.42 10 7 3 444.89 22.75 -10 -7 -3 451.74 26.42 10 7 3 450.01 24.28 10 7 3 391.65 22.84 10 7 4 475.13 23.91 -10 -7 -4 441.71 25.39 10 7 4 461.73 23.20 10 7 4 441.13 23.82 10 7 5 2.67 4.90 -10 -7 -5 6.06 5.64 10 7 5 9.08 6.33 10 7 6 65.02 9.13 -10 -7 -6 64.31 9.76 10 7 6 59.09 9.19 -10 7 -7 105.81 12.17 10 7 7 107.36 11.41 -10 -7 -7 121.20 11.76 10 7 7 109.14 10.92 10 7 8 428.40 18.93 -10 -7 -8 458.54 20.14 10 7 8 457.98 19.08 -10 -7 -9 3.01 3.33 10 7 9 8.46 3.91 -10 -7 -9 10.57 3.92 10 7 9 13.10 3.39 10 -8 -14 4.39 2.03 10 -8 -13 -2.43 3.40 10 -8 -13 2.29 4.36 10 -8 -12 20.20 4.94 10 -8 -12 8.52 6.51 10 -8 -11 668.05 28.50 10 -8 -11 708.47 29.96 10 -8 -10 121.48 14.32 10 -8 -10 120.13 13.03 10 -8 -10 125.80 13.79 10 -8 -9 200.91 19.08 10 -8 -9 200.28 17.83 10 8 -9 225.76 17.40 10 -8 -9 193.82 17.33 10 -8 -8 55.35 13.24 10 -8 -8 69.65 11.87 10 8 -8 65.17 11.02 10 -8 -8 58.89 9.88 10 -8 -7 265.46 21.36 10 8 -7 249.47 19.77 10 -8 -7 248.72 20.19 10 -8 -6 12.02 7.19 10 -8 -6 9.77 5.20 10 8 -6 3.26 6.01 10 8 -5 506.13 29.23 10 -8 -5 453.82 25.94 10 -8 -4 226.25 18.88 10 8 -4 221.35 19.53 10 -8 -4 193.90 16.58 -10 -8 3 42.88 11.23 10 -8 -3 45.18 9.17 10 8 -3 42.84 10.58 -10 -8 2 14.17 9.55 10 -8 -2 29.70 8.74 10 8 -2 2.94 7.10 -10 -8 1 295.54 23.09 10 -8 -1 275.90 19.54 10 8 -1 262.78 17.78 10 8 -1 310.42 22.59 -10 -8 0 270.73 20.71 10 8 0 216.93 15.93 10 8 0 259.54 20.53 -10 -8 -1 448.29 25.65 10 8 1 419.18 24.82 10 8 1 369.15 20.86 -10 -8 -2 65.22 10.59 10 8 2 89.40 11.39 10 8 2 80.68 9.97 -10 -8 -3 14.80 6.99 10 8 3 16.79 6.04 10 8 3 4.04 3.86 10 8 4 65.62 7.78 -10 -8 -4 66.67 10.62 10 8 4 66.71 8.27 10 8 4 64.39 9.00 10 8 5 340.61 17.91 -10 -8 -5 355.39 20.11 10 8 5 333.49 18.04 10 8 6 3.65 3.68 -10 -8 -6 4.52 4.69 10 8 6 8.39 4.38 10 8 7 105.59 9.51 -10 -8 -7 109.02 10.07 10 8 7 101.72 9.50 -10 -8 -7 87.56 9.03 10 8 8 94.06 8.42 -10 -8 -8 86.52 8.18 10 8 8 79.35 7.42 -10 -8 -8 81.80 7.58 10 -9 -13 11.33 4.85 10 -9 -12 258.48 16.25 10 -9 -11 12.11 6.27 10 -9 -10 172.81 14.71 10 -9 -9 36.26 9.02 10 9 -9 20.37 5.37 10 -9 -8 567.44 27.25 10 9 -8 562.45 25.88 10 -9 -7 21.01 7.95 10 -9 -7 25.03 6.44 10 9 -7 19.81 6.59 10 -9 -6 33.22 8.25 10 -9 -6 35.76 8.16 10 9 -6 45.78 9.43 10 -9 -5 4.70 5.98 10 -9 -5 -10.54 4.88 10 9 -5 6.56 5.31 -10 -9 4 336.57 23.01 10 9 -4 366.58 23.48 -10 -9 3 5.75 8.18 10 -9 -3 0.20 2.27 10 9 -3 12.37 8.07 -10 -9 2 324.80 22.10 10 9 -2 327.78 22.57 -10 -9 1 4.84 5.26 10 9 -1 2.51 2.71 -10 -9 0 13.25 7.07 10 9 0 15.69 5.37 10 9 0 20.33 7.39 -10 -9 -1 9.22 6.28 10 9 1 14.08 5.33 10 9 1 11.30 4.26 -10 -9 -2 396.63 22.20 10 9 2 423.85 21.55 10 9 2 376.11 18.58 -10 -9 -3 9.66 5.71 10 9 3 6.30 4.31 10 9 3 -0.51 4.29 -10 -9 -4 446.95 21.51 10 9 4 429.33 19.18 10 9 5 -1.82 2.83 -10 -9 -5 2.47 4.31 10 9 5 3.00 3.82 10 9 6 6.29 3.48 -10 -9 -6 13.05 3.13 10 9 6 4.80 2.86 -10 -9 -7 -4.50 2.64 10 9 7 3.48 2.53 10 -10 -12 23.66 5.50 10 -10 -11 470.95 20.15 10 -10 -10 4.29 4.36 10 10 -9 113.02 10.23 10 -10 -9 97.85 10.66 10 -10 -8 13.20 5.25 10 10 -8 14.64 3.80 -10 -10 7 166.65 14.45 10 10 -7 169.31 14.18 10 -10 -7 150.42 13.25 10 -10 -6 1.37 5.14 -10 -10 6 1.48 5.60 10 10 -6 -0.41 5.65 -10 -10 5 537.72 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19.72 12 5 -3 207.83 16.84 -12 -5 2 12.15 6.17 12 -5 -2 4.04 2.07 12 5 -2 9.35 4.60 12 5 -2 4.13 3.29 -12 -5 1 52.19 11.57 12 5 -1 52.74 9.51 12 -5 -1 42.61 8.93 12 5 -1 43.95 8.74 -12 -5 0 243.37 19.06 12 -5 0 224.19 17.83 12 5 0 263.08 19.21 12 5 0 231.30 17.70 -12 -5 -1 332.54 21.55 12 -5 1 313.83 20.24 12 5 1 338.81 20.63 12 5 1 351.05 20.63 -12 -5 -2 275.03 18.48 12 5 2 265.24 17.28 12 -5 2 234.81 16.51 12 5 2 276.51 18.43 -12 -5 -3 14.04 7.29 12 5 3 27.99 6.87 12 5 3 20.93 5.16 -12 -5 -4 34.87 6.77 12 5 4 24.27 6.93 -12 -5 -5 102.77 9.43 12 5 5 101.10 9.80 -12 -5 -6 409.40 16.65 12 5 6 436.82 17.81 12 -6 -13 165.42 11.91 12 -6 -12 129.33 12.22 12 -6 -12 124.01 11.48 12 -6 -11 84.71 11.52 12 -6 -11 80.24 11.44 12 -6 -11 82.57 10.82 12 -6 -10 64.20 11.04 12 -6 -10 72.35 12.28 12 6 -10 68.92 8.11 12 -6 -10 62.50 10.19 12 -6 -9 -1.18 8.35 12 -6 -9 9.74 6.39 12 6 -9 1.15 5.78 12 -6 -9 4.04 5.69 12 -6 -8 21.14 6.29 12 6 -8 12.01 6.27 12 -6 -8 14.85 5.98 12 -6 -7 204.24 18.63 12 6 -7 188.93 16.52 12 -6 -7 181.98 16.41 12 -6 -6 114.43 14.67 12 6 -6 110.97 13.40 12 -6 -6 107.87 12.82 -12 -6 5 99.42 13.97 12 -6 -5 108.44 14.72 12 6 -5 93.82 13.77 -12 -6 4 3.63 7.02 12 -6 -4 -4.89 3.98 12 6 -4 5.32 2.54 12 6 -4 3.21 5.80 -12 -6 3 81.41 13.18 12 -6 -3 92.15 11.69 12 6 -3 91.06 12.63 12 6 -3 85.20 10.68 -12 -6 2 88.96 12.11 12 -6 -2 101.66 11.85 12 6 -2 87.75 12.46 12 6 -2 68.69 9.43 -12 -6 1 716.70 31.00 12 -6 -1 629.83 28.36 12 6 -1 707.04 30.95 12 6 -1 641.40 26.26 -12 -6 0 15.42 4.11 12 -6 0 -1.77 3.08 12 6 0 11.41 3.65 12 6 0 1.56 4.36 -12 -6 -1 18.18 7.35 12 6 1 5.25 6.12 12 6 1 17.95 5.11 -12 -6 -2 135.76 13.77 12 6 2 132.05 11.20 12 6 2 115.76 11.33 -12 -6 -3 770.53 27.42 12 6 3 719.87 23.98 12 6 3 710.01 25.50 -12 -6 -4 160.50 12.52 12 6 4 142.84 11.34 -12 -6 -5 159.70 11.68 12 6 5 146.46 10.65 12 6 6 5.60 2.80 12 -7 -12 19.77 5.59 12 -7 -11 -2.40 3.86 12 -7 -10 138.68 13.45 12 -7 -10 122.61 11.83 12 -7 -9 3.11 2.87 12 7 -9 5.17 4.36 12 -7 -9 1.47 4.22 12 -7 -8 99.11 12.48 12 7 -8 111.51 11.74 12 -7 -8 94.39 11.49 12 -7 -7 6.20 3.82 12 7 -7 2.68 3.72 12 -7 -7 3.39 5.17 -12 -7 6 144.42 14.20 12 -7 -6 157.45 15.73 12 7 -6 143.24 13.67 -12 -7 5 14.98 8.72 12 -7 -5 12.35 3.93 12 7 -5 12.71 6.47 -12 -7 4 450.35 24.31 12 -7 -4 423.54 23.73 12 7 -4 428.75 24.00 -12 -7 3 160.31 14.61 12 -7 -3 176.61 14.85 12 7 -3 172.36 14.94 -12 -7 2 9.59 7.89 12 -7 -2 10.55 5.10 12 7 -2 8.66 5.28 12 7 -2 20.13 5.36 -12 -7 1 27.74 7.42 12 -7 -1 23.26 7.10 12 7 -1 33.47 5.87 12 7 -1 23.00 5.76 -12 -7 0 392.84 21.24 12 7 0 385.52 20.49 12 7 0 338.81 17.70 -12 -7 -1 338.87 19.04 12 7 1 364.43 18.38 12 7 1 312.95 16.45 -12 -7 -2 328.36 18.24 12 7 2 322.43 16.19 12 7 2 275.31 15.37 -12 -7 -3 126.62 11.03 12 7 3 118.56 10.13 -12 -7 -4 56.30 7.14 12 7 4 51.98 6.56 -12 -7 -5 35.62 5.20 12 7 5 30.61 4.78 12 -8 -11 400.49 17.66 12 -8 -10 26.40 4.88 12 8 -9 32.57 6.15 12 -8 -9 22.54 6.09 -12 -8 8 16.56 5.74 12 -8 -8 22.60 4.87 12 8 -8 20.75 5.56 12 -8 -8 25.32 5.66 -12 -8 7 556.54 23.92 12 -8 -7 618.51 26.37 12 8 -7 571.74 23.18 12 -8 -7 511.03 22.80 -12 -8 6 5.93 6.78 12 -8 -6 9.49 4.75 12 8 -6 13.63 3.53 -12 -8 5 25.39 6.85 12 -8 -5 28.24 5.39 12 8 -5 24.69 6.63 -12 -8 4 15.64 5.28 12 -8 -4 20.18 4.37 12 8 -4 20.65 6.73 -12 -8 3 327.02 18.31 12 8 -3 342.95 19.52 -12 -8 2 5.00 4.44 12 8 -2 10.53 3.73 -12 -8 1 322.77 17.86 12 8 -1 332.17 18.03 12 8 -1 272.70 12.99 -12 -8 0 11.43 4.48 12 8 0 5.56 2.82 12 8 0 0.99 3.15 -12 -8 -1 107.61 9.78 12 8 1 104.45 9.07 12 8 1 92.89 7.91 -12 -8 -2 4.47 3.51 12 8 2 1.85 2.58 -12 -8 -3 384.60 16.27 12 8 3 339.09 13.59 -12 -9 9 7.10 3.72 -12 -9 8 69.73 7.66 -12 -9 7 9.78 4.85 12 9 -7 8.82 4.02 -12 -9 6 517.18 20.87 12 9 -6 571.12 21.63 -12 -9 5 11.65 4.62 12 9 -5 13.68 4.55 -12 -9 4 420.92 18.65 12 9 -4 452.87 19.99 -12 -9 3 6.25 3.67 12 9 -3 12.31 3.55 -12 -9 2 -2.29 1.75 12 9 -2 5.84 3.27 -12 -9 1 15.07 4.80 12 9 -1 10.41 3.17 -12 -9 0 179.87 11.37 12 9 0 263.30 13.15 -12 -9 -1 11.34 3.26 12 10 -4 4.74 2.30 12 10 -3 371.56 15.10 13 0 -13 227.84 12.80 13 0 -12 -11.44 4.43 13 0 -11 651.19 23.49 13 0 -11 467.44 21.37 13 0 -10 13.17 3.82 13 0 -10 5.06 5.77 13 0 -9 151.12 12.68 13 0 -9 163.37 15.51 13 0 -8 -1.89 4.49 13 0 -7 144.77 15.96 13 0 -6 10.31 7.05 13 0 -5 591.52 33.29 13 0 -5 653.83 33.67 13 0 -4 7.76 7.13 13 0 -4 5.31 6.84 13 0 -3 119.93 14.56 13 0 -3 138.74 17.05 13 0 -2 -2.95 8.21 13 0 -1 125.99 15.08 13 0 0 16.21 5.02 13 0 1 439.86 24.45 13 0 2 -6.03 5.40 13 0 3 5.39 2.97 -13 0 -4 12.58 4.53 13 0 4 2.73 1.87 -13 0 -5 496.59 20.69 13 0 5 491.47 18.74 13 -1 -13 89.32 9.25 13 -1 -12 364.61 18.13 13 -1 -12 344.95 17.00 13 -1 -11 48.65 7.84 13 -1 -11 49.45 7.73 13 -1 -10 10.09 4.34 13 -1 -10 6.00 5.13 13 1 -10 8.28 3.49 13 -1 -9 76.60 10.48 13 -1 -9 84.05 12.17 13 1 -9 94.98 10.93 13 1 -8 432.38 27.92 13 -1 -8 437.00 26.85 13 1 -8 414.15 23.55 13 1 -7 153.12 17.66 13 -1 -7 149.31 16.73 13 1 -7 157.11 16.04 13 1 -6 62.84 12.01 13 -1 -6 56.85 11.01 13 1 -6 50.67 10.48 13 -1 -5 32.26 9.89 13 1 -5 30.70 8.24 13 1 -5 31.03 9.29 13 1 -4 187.59 18.69 13 -1 -4 215.27 20.30 13 1 -4 207.26 19.76 13 1 -3 106.66 14.16 13 -1 -3 102.94 15.19 13 1 -3 126.90 15.65 13 1 -2 618.38 30.82 13 -1 -2 716.75 34.93 13 1 -2 657.96 32.26 13 -1 -1 12.92 4.51 13 1 -1 1.73 7.85 13 1 -1 7.26 4.36 13 -1 0 9.92 3.59 13 1 0 5.55 5.75 13 1 0 13.26 5.98 13 -1 1 109.45 11.72 13 1 1 108.51 11.76 13 -1 2 732.08 29.00 13 1 2 742.81 29.79 -13 1 -3 20.27 4.99 13 -1 3 21.66 4.36 13 1 3 28.73 6.37 -13 1 -4 392.05 18.67 13 -1 4 418.81 19.00 13 1 4 418.69 19.70 -13 1 -5 23.43 5.46 -13 -1 -5 28.48 4.90 13 1 5 39.74 5.85 13 -2 -13 82.31 8.53 13 -2 -12 26.05 6.63 13 -2 -12 31.95 7.09 13 -2 -11 556.74 23.68 13 -2 -11 572.73 26.23 13 -2 -10 252.07 17.37 13 -2 -10 271.48 20.24 13 -2 -9 244.92 17.81 13 2 -9 250.95 19.88 13 -2 -9 246.02 20.44 13 -2 -8 3.50 7.42 13 2 -8 1.41 2.41 13 2 -8 1.91 3.60 13 2 -7 367.03 25.60 13 -2 -7 336.71 25.51 13 2 -7 329.94 21.03 -13 -2 6 232.93 18.14 13 2 -6 291.34 22.42 13 -2 -6 302.19 24.67 13 2 -6 318.88 21.51 -13 -2 5 661.63 28.88 13 2 -5 727.48 34.50 13 -2 -5 736.26 37.35 13 2 -5 705.60 32.43 -13 -2 4 52.00 9.28 13 2 -4 60.70 10.93 13 -2 -4 43.20 10.65 13 2 -4 45.88 10.67 -13 -2 3 25.66 7.20 13 -2 -3 30.85 10.28 13 2 -3 22.76 8.31 13 2 -3 19.41 7.87 -13 -2 2 47.01 7.15 13 -2 -2 34.95 9.62 13 2 -2 46.14 9.67 13 2 -2 47.09 9.14 -13 -2 1 350.47 19.52 13 2 -1 393.97 24.06 13 2 -1 378.90 23.60 13 2 0 76.70 10.78 13 -2 0 83.27 12.03 13 2 0 84.69 11.64 13 2 1 362.40 21.16 13 -2 1 392.07 22.88 13 2 1 380.33 21.88 13 -2 2 11.77 5.42 13 2 2 15.17 6.10 13 -2 3 79.67 9.26 13 2 3 94.99 10.71 13 -2 4 77.89 8.39 13 2 4 96.92 9.67 13 2 5 336.58 15.77 13 -3 -13 69.16 7.68 13 -3 -12 272.68 16.08 13 -3 -12 286.77 16.69 13 -3 -11 21.94 7.57 13 -3 -11 29.48 7.87 13 -3 -10 8.00 5.78 13 -3 -10 -0.03 5.49 13 -3 -9 119.72 13.18 13 3 -9 145.23 14.58 13 -3 -9 124.00 15.02 13 3 -8 354.60 23.57 13 -3 -8 340.76 24.66 13 3 -8 342.10 18.31 13 3 -7 182.98 17.94 13 -3 -7 182.38 19.39 13 3 -7 196.56 15.05 -13 -3 6 66.32 10.83 13 3 -6 55.45 9.73 13 -3 -6 65.91 12.69 13 3 -6 52.31 10.19 -13 -3 5 35.77 9.31 13 3 -5 47.60 9.39 13 -3 -5 54.77 12.14 13 3 -5 51.08 10.17 -13 -3 4 424.06 23.25 13 3 -4 493.13 27.79 13 -3 -4 521.16 30.13 13 3 -4 470.62 24.93 13 3 -3 218.66 18.57 13 -3 -3 246.27 20.19 13 3 -3 206.59 16.87 -13 -3 2 299.25 18.25 13 3 -2 334.98 22.54 13 -3 -2 345.58 23.54 13 3 -2 311.19 20.07 -13 -3 1 -7.47 6.04 13 -3 -1 5.15 7.13 13 3 -1 2.17 5.74 13 3 -1 6.29 4.72 -13 -3 0 219.12 14.98 13 3 0 281.84 18.94 13 -3 0 265.53 19.93 13 3 0 262.24 17.96 -13 -3 -1 216.49 14.23 13 3 1 230.90 16.15 13 -3 1 248.05 17.48 13 3 1 229.32 16.69 13 3 2 461.34 21.01 13 -3 2 472.40 21.39 13 3 2 477.40 23.09 -13 -3 -3 77.48 7.88 13 -3 3 89.86 8.94 13 3 3 107.00 10.55 13 3 4 11.38 3.58 13 3 5 5.69 2.93 13 -4 -13 4.42 3.75 13 -4 -12 112.82 10.83 13 -4 -12 106.26 10.19 13 -4 -11 598.79 23.89 13 -4 -11 611.75 27.04 13 -4 -10 41.04 8.76 13 4 -10 57.82 7.96 13 -4 -10 56.89 10.11 13 -4 -9 252.55 20.42 13 4 -9 292.66 18.45 13 -4 -8 9.08 6.25 13 4 -8 -6.97 6.23 13 -4 -7 437.15 27.50 13 4 -7 448.80 24.93 -13 -4 6 224.08 17.66 13 -4 -6 288.78 21.77 13 4 -6 241.03 19.58 13 4 -6 250.16 16.30 -13 -4 5 737.29 30.61 13 -4 -5 818.37 36.58 13 4 -5 763.03 32.72 13 4 -5 751.81 28.30 -13 -4 4 84.39 11.35 13 -4 -4 95.58 13.51 13 4 -4 83.15 12.68 13 4 -4 90.96 10.33 -13 -4 3 6.13 5.57 13 -4 -3 13.72 3.98 13 4 -3 12.53 5.16 13 4 -3 6.23 3.17 -13 -4 2 15.10 4.16 13 -4 -2 12.08 5.44 13 4 -2 21.33 6.82 13 4 -2 18.47 5.98 -13 -4 1 480.28 22.50 13 4 -1 515.90 25.43 13 -4 -1 473.73 25.23 13 4 -1 452.42 22.75 -13 -4 0 107.18 11.38 13 4 0 123.20 12.42 13 -4 0 116.61 12.11 13 4 0 104.24 11.88 -13 -4 -1 75.02 8.93 13 4 1 75.72 8.91 13 -4 1 61.70 7.85 13 4 1 68.96 8.96 -13 -4 -2 9.73 3.06 13 -4 2 3.74 3.36 13 4 2 6.84 4.48 13 4 2 9.79 3.66 -13 -4 -3 54.16 6.42 13 4 3 74.96 8.79 13 4 4 260.93 14.57 13 4 5 241.49 11.98 13 -5 -11 18.31 5.49 13 -5 -10 8.65 6.25 13 5 -9 53.88 8.04 13 -5 -9 43.97 9.67 13 -5 -8 197.76 17.38 13 5 -8 186.79 14.73 -13 -5 7 37.22 9.04 13 -5 -7 35.79 7.50 13 5 -7 30.77 6.44 -13 -5 6 -6.06 6.85 13 -5 -6 2.59 5.24 13 5 -6 2.25 5.30 -13 -5 5 18.99 6.88 13 -5 -5 18.12 5.42 13 5 -5 -2.00 2.92 13 5 -5 13.73 6.31 -13 -5 4 241.23 16.77 13 -5 -4 250.56 18.97 13 5 -4 232.93 18.18 13 5 -4 227.96 14.26 -13 -5 3 50.44 8.60 13 -5 -3 50.33 8.26 13 5 -3 44.58 8.31 13 5 -3 50.47 7.52 -13 -5 2 113.99 11.45 13 -5 -2 92.89 11.35 13 5 -2 121.17 12.36 13 5 -2 107.22 10.49 -13 -5 1 24.47 7.03 13 -5 -1 17.72 6.07 13 5 -1 27.18 6.19 13 5 -1 23.62 6.40 -13 -5 0 103.36 9.97 13 5 0 92.82 10.22 13 -5 0 91.21 10.70 13 5 0 92.41 10.00 -13 -5 -1 33.32 6.50 13 5 1 36.50 6.48 13 -5 1 26.72 4.51 13 5 1 28.89 5.26 -13 -5 -2 478.84 18.89 13 5 2 436.49 17.56 13 5 2 475.07 19.81 -13 -5 -3 320.69 14.87 13 5 3 354.12 16.07 13 5 4 18.65 3.89 13 -6 -10 72.30 8.85 -13 -6 9 12.03 5.43 13 -6 -9 6.26 4.30 13 6 -9 8.70 4.23 -13 -6 8 65.76 9.09 13 -6 -8 76.01 9.73 13 6 -8 67.98 8.38 -13 -6 7 40.74 7.52 13 -6 -7 47.94 8.17 13 6 -7 38.47 7.13 -13 -6 6 372.61 20.05 13 -6 -6 380.38 21.85 13 6 -6 381.27 20.47 -13 -6 5 133.31 12.72 13 -6 -5 117.86 12.00 13 6 -5 134.98 13.64 -13 -6 4 108.39 11.58 13 -6 -4 113.59 11.31 13 6 -4 105.74 12.12 -13 -6 3 48.04 8.61 13 -6 -3 47.00 7.27 13 6 -3 51.06 7.27 13 6 -3 42.99 5.45 -13 -6 2 41.39 6.45 13 -6 -2 32.67 5.29 13 6 -2 31.94 5.92 13 6 -2 35.76 7.20 -13 -6 1 31.39 6.53 13 -6 -1 30.14 4.84 13 6 -1 16.63 4.89 13 6 -1 26.15 6.30 -13 -6 0 282.55 15.76 13 6 0 271.92 15.61 13 6 0 243.69 13.81 -13 -6 -1 76.95 8.28 13 6 1 77.34 8.15 13 6 1 72.31 7.80 -13 -6 -2 23.23 4.94 13 6 2 18.34 4.45 13 6 3 8.97 3.21 -13 -7 9 148.91 10.93 13 -7 -9 129.45 10.40 -13 -7 8 20.83 5.60 13 -7 -8 11.02 4.47 13 7 -8 21.82 4.03 -13 -7 7 199.71 13.39 13 -7 -7 190.63 13.93 13 7 -7 202.66 13.05 -13 -7 6 2.61 3.86 13 -7 -6 -4.56 2.95 13 7 -6 -0.18 4.61 -13 -7 5 30.15 6.81 13 -7 -5 33.08 6.03 13 7 -5 24.60 6.33 -13 -7 4 9.52 5.75 13 -7 -4 2.73 2.38 13 7 -4 5.73 3.14 -13 -7 3 186.55 13.23 13 7 -3 191.35 13.22 -13 -7 2 8.29 5.24 13 7 -2 7.97 3.84 -13 -7 1 78.98 8.33 13 7 -1 76.56 8.08 13 7 -1 59.68 6.55 -13 -7 0 2.74 3.81 13 7 0 -8.45 3.27 -13 -7 -1 130.77 9.06 -13 -8 7 5.20 3.54 -13 -8 6 491.42 18.06 13 8 -6 503.44 18.70 -13 -8 5 7.80 2.99 13 8 -5 9.79 4.45 -13 -8 4 269.98 13.63 13 8 -4 299.72 14.84 -13 -8 3 33.96 5.56 13 8 -3 32.57 5.36 -13 -8 2 138.16 9.68 13 8 -2 136.20 9.59 -13 -8 1 2.99 3.39 14 0 -10 211.28 12.66 14 0 -9 2.02 2.93 14 0 -8 48.79 7.99 14 0 -7 5.35 3.61 14 0 -6 218.69 16.97 14 0 -5 4.30 5.32 14 0 -4 206.32 16.57 14 0 -3 6.83 5.93 14 0 -2 23.77 6.65 14 0 -1 3.98 1.98 14 0 0 206.02 14.22 14 0 1 1.85 2.96 14 0 2 777.88 23.95 14 -1 -10 52.34 7.32 14 -1 -9 22.40 5.12 14 1 -9 30.14 5.12 14 -1 -8 4.90 4.70 14 1 -8 11.12 5.11 14 -1 -7 603.04 26.35 14 1 -7 574.49 24.11 14 -1 -6 58.78 10.25 14 1 -6 66.73 9.25 14 -1 -5 287.52 19.68 14 1 -5 279.94 18.24 14 -1 -4 7.99 5.77 14 1 -4 7.59 5.80 14 -1 -3 54.13 9.29 14 1 -3 48.34 8.94 14 -1 -2 93.47 11.15 14 1 -2 98.16 10.63 14 -1 -1 403.48 20.93 14 1 -1 383.79 19.69 14 1 0 39.66 6.80 14 -1 0 26.38 5.99 14 -1 1 3.27 1.91 14 1 1 4.94 2.15 14 -1 2 60.91 7.32 14 1 2 67.57 6.97 14 -2 -10 103.33 9.72 14 -2 -9 65.52 9.07 14 -2 -8 192.71 15.76 14 2 -8 177.95 11.40 14 -2 -7 56.71 9.68 14 2 -7 54.80 7.34 14 2 -6 40.93 6.66 14 -2 -6 40.42 9.16 14 2 -5 70.00 9.95 14 -2 -5 90.79 11.41 14 2 -5 78.41 9.50 14 2 -4 367.89 20.98 14 -2 -4 414.46 22.68 14 2 -4 373.35 19.38 14 2 -3 106.53 11.38 14 -2 -3 112.31 12.01 14 2 -3 93.30 10.79 14 -2 -2 34.78 6.26 14 2 -2 38.08 7.30 14 -2 -1 58.31 8.62 14 2 -1 68.33 8.77 14 -2 0 347.72 17.52 14 2 0 331.68 17.56 14 -2 1 195.27 11.86 14 2 1 222.52 13.52 14 2 2 664.95 21.65 14 -3 -10 129.59 11.31 14 -3 -9 36.06 6.24 -14 -3 8 4.72 2.24 14 -3 -8 4.14 5.22 -14 -3 7 711.55 22.51 14 3 -7 803.34 28.14 14 -3 -7 841.93 31.28 14 3 -7 717.49 21.41 -14 -3 6 124.45 10.18 14 3 -6 146.17 12.99 14 -3 -6 145.04 14.14 14 3 -6 128.85 10.35 -14 -3 5 346.59 16.34 14 3 -5 392.01 21.07 14 -3 -5 414.96 22.38 14 3 -5 358.24 17.28 -14 -3 4 19.24 4.69 14 -3 -4 15.69 5.75 14 3 -4 11.53 5.00 14 3 -4 9.85 3.44 -14 -3 3 52.30 7.33 14 3 -3 72.88 8.88 14 -3 -3 75.23 10.14 14 3 -3 62.86 8.06 14 3 -2 121.97 11.18 14 -3 -2 99.30 10.88 14 3 -2 120.51 11.10 14 -3 -1 370.70 18.07 14 3 -1 366.18 17.55 14 3 0 43.09 6.68 14 -3 0 24.13 5.67 14 3 1 6.03 3.01 14 3 2 31.65 5.36 14 -4 -10 69.61 8.30 14 -4 -9 53.84 8.18 -14 -4 8 266.50 13.55 14 4 -8 303.42 15.52 14 -4 -8 301.77 17.88 -14 -4 7 5.98 2.84 14 -4 -7 6.65 4.74 14 4 -7 4.48 3.23 -14 -4 6 55.40 7.87 14 4 -6 68.48 8.61 14 -4 -6 68.59 8.99 -14 -4 5 42.92 6.28 14 4 -5 44.78 7.63 14 -4 -5 45.19 7.86 14 4 -5 33.01 5.84 -14 -4 4 537.61 19.56 14 4 -4 593.91 23.99 14 -4 -4 602.77 24.88 14 4 -4 551.66 19.34 -14 -4 3 52.29 7.13 14 4 -3 53.09 8.33 14 -4 -3 58.27 7.45 14 4 -3 45.80 6.59 -14 -4 2 29.25 5.57 14 4 -2 49.01 6.75 14 -4 -2 49.16 6.66 14 4 -2 38.67 6.52 14 -4 -1 5.70 3.15 14 4 -1 2.98 3.31 14 4 -1 6.20 3.83 14 4 0 456.54 17.55 14 4 1 102.38 8.68 14 -5 -8 94.62 9.54 -14 -5 7 246.91 12.89 14 5 -7 233.46 13.55 -14 -5 6 103.36 9.09 14 -5 -6 101.30 10.21 -14 -5 5 204.11 12.34 14 -5 -5 223.55 14.12 14 5 -5 224.13 13.95 -14 -5 4 4.56 3.16 14 -5 -4 3.92 2.84 14 5 -4 5.84 3.60 -14 -5 3 43.52 6.10 14 5 -3 45.87 6.08 14 -5 -3 39.94 6.03 14 5 -2 87.50 8.35 14 5 -2 71.06 7.18 14 5 -1 219.18 12.14 14 6 -5 113.13 9.40 14 6 -4 81.08 7.93 14 6 -3 62.49 6.91 15 0 -5 15.71 4.00 15 0 -4 0.33 2.16 15 0 -3 292.88 13.90 15 -1 -5 40.79 6.07 15 -1 -4 105.36 9.39 15 -1 -3 1.14 3.50 0 0 0 0.00 0.00 TITL GARD25Y in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 12.331430 13.537080 17.361036 90.0000 102.9286 90.0000 ZERR 4.00 0.000178 0.000177 0.000262 0.0000 0.0014 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O P Br Re UNIT 120.00 100.00 16.00 12.00 4.00 4.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 40765 _olex2_submission_original_sample_id gard25y _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 1.659 _oxdiff_exptl_absorpt_empirical_full_min 0.634 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Re1 Re 0.59843(2) 0.47283(2) 0.34669(2) 0.01755(7) Uani 1 1 d . . . . . Br1A Br 0.49653(6) 0.63429(7) 0.37173(4) 0.01993(15) Uani 0.8 1 d . . P A 1 Br1B Br 0.6772(3) 0.3002(4) 0.3465(3) 0.0277(10) Uani 0.2 1 d . . P A -1 P1 P 0.54117(8) 0.48965(7) 0.20043(6) 0.0161(2) Uani 1 1 d . . . . . O3 O 0.6943(3) 0.4637(2) 0.52756(19) 0.0346(8) Uani 1 1 d . . . . . O1 O 0.8164(3) 0.5755(3) 0.3358(2) 0.0376(8) Uani 1 1 d . . . . . O2A O 0.6963(7) 0.2650(6) 0.3365(5) 0.036(2) Uani 0.8 1 d . . P A 1 O2B O 0.4815(18) 0.6657(15) 0.3733(12) 0.018(6) Uiso 0.2 1 d . . P A -1 N11 N 0.3372(3) 0.4103(2) 0.31819(19) 0.0190(7) Uani 1 1 d . . . . . N12 N 0.4448(3) 0.3962(2) 0.35839(19) 0.0177(7) Uani 1 1 d . . . . . N21 N 0.2093(3) 0.5246(2) 0.2414(2) 0.0199(7) Uani 1 1 d . . . . . N22 N 0.1084(3) 0.4779(3) 0.2262(3) 0.0303(9) Uani 1 1 d . . . . . C1 C 0.4240(3) 0.4119(3) 0.1501(2) 0.0185(8) Uani 1 1 d . . . . . C2 C 0.3231(3) 0.4106(3) 0.1757(2) 0.0169(8) Uani 1 1 d . . . . . C3 C 0.2380(3) 0.3478(3) 0.1390(2) 0.0205(8) Uani 1 1 d . . . . . H3 H 0.171756 0.346468 0.156056 0.025 Uiso 1 1 calc R U . . . C4 C 0.2507(3) 0.2872(3) 0.0773(3) 0.0247(9) Uani 1 1 d . . . . . H4 H 0.193161 0.245241 0.053553 0.030 Uiso 1 1 calc R U . . . C5 C 0.3487(3) 0.2889(3) 0.0508(2) 0.0252(9) Uani 1 1 d . . . . . H5 H 0.357060 0.248342 0.009303 0.030 Uiso 1 1 calc R U . . . C6 C 0.4343(3) 0.3515(3) 0.0868(2) 0.0215(8) Uani 1 1 d . . . . . H6 H 0.499585 0.353366 0.068508 0.026 Uiso 1 1 calc R U . . . C7 C 0.3128(3) 0.4725(3) 0.2465(2) 0.0179(8) Uani 1 1 d . . . . . H7 H 0.371525 0.522678 0.253276 0.021 Uiso 1 1 calc R U . . . C10 C 0.6547(4) 0.4666(3) 0.4625(3) 0.0232(9) Uani 1 1 d . . . . . C8 C 0.7344(4) 0.5380(3) 0.3393(2) 0.0244(9) Uani 1 1 d . . . . . C9A C 0.6604(7) 0.3458(6) 0.3361(5) 0.0257(19) Uani 0.8 1 d . . P A 1 C9B C 0.527(2) 0.601(2) 0.3684(16) 0.025(8) Uiso 0.2 1 d . . P A -1 C11 C 0.2677(3) 0.3496(3) 0.3446(3) 0.0253(9) Uani 1 1 d . . . . . H11 H 0.191277 0.344669 0.325086 0.030 Uiso 1 1 calc R U . . . C12 C 0.3306(4) 0.2959(4) 0.4060(3) 0.0298(10) Uani 1 1 d . . . . . H12 H 0.305632 0.248695 0.436928 0.036 Uiso 1 1 calc R U . . . C13 C 0.4386(4) 0.3271(3) 0.4117(3) 0.0260(9) Uani 1 1 d . . . . . H13 H 0.499588 0.302829 0.448316 0.031 Uiso 1 1 calc R U . . . C21 C 0.1999(4) 0.6211(3) 0.2590(3) 0.0316(10) Uani 1 1 d . . . . . H21 H 0.257622 0.666534 0.271986 0.038 Uiso 1 1 calc R U . . . C22 C 0.0902(4) 0.6390(4) 0.2544(3) 0.0388(12) Uani 1 1 d . . . . . H22 H 0.057411 0.698652 0.263003 0.047 Uiso 1 1 calc R U . . . C23 C 0.0377(4) 0.5492(4) 0.2339(3) 0.0303(10) Uani 1 1 d . . . . . H23 H -0.038689 0.539832 0.226478 0.036 Uiso 1 1 calc R U . . . C31 C 0.6545(3) 0.4604(3) 0.1511(2) 0.0184(8) Uani 1 1 d . . . . . C32 C 0.6979(3) 0.5316(3) 0.1087(3) 0.0227(9) Uani 1 1 d . . . . . H32 H 0.666721 0.594504 0.103214 0.027 Uiso 1 1 calc R U . . . C33 C 0.7860(3) 0.5111(3) 0.0745(3) 0.0231(9) Uani 1 1 d . . . . . H33 H 0.813072 0.560167 0.046338 0.028 Uiso 1 1 calc R U . . . C34 C 0.8353(3) 0.4173(3) 0.0817(2) 0.0196(8) Uani 1 1 d . . . . . C35 C 0.7918(3) 0.3466(3) 0.1241(2) 0.0211(8) Uani 1 1 d . . . . . H35 H 0.822770 0.283632 0.129362 0.025 Uiso 1 1 calc R U . . . C36 C 0.7039(3) 0.3669(3) 0.1588(2) 0.0218(9) Uani 1 1 d . . . . . H36 H 0.677396 0.318004 0.187415 0.026 Uiso 1 1 calc R U . . . C37 C 0.9320(3) 0.3970(3) 0.0450(3) 0.0246(9) Uani 1 1 d . . . . . H37A H 0.994418 0.436446 0.070580 0.037 Uiso 1 1 calc R U . . . H37B H 0.912221 0.413064 -0.010184 0.037 Uiso 1 1 calc R U . . . H37C H 0.951467 0.328283 0.051239 0.037 Uiso 1 1 calc R U . . . C41 C 0.5019(3) 0.6134(3) 0.1617(2) 0.0176(8) Uani 1 1 d . . . . . C42 C 0.4278(3) 0.6276(3) 0.0895(2) 0.0195(8) Uani 1 1 d . . . . . H42 H 0.388004 0.574285 0.063553 0.023 Uiso 1 1 calc R U . . . C43 C 0.4130(3) 0.7209(3) 0.0561(2) 0.0213(8) Uani 1 1 d . . . . . H43 H 0.363426 0.729240 0.007665 0.026 Uiso 1 1 calc R U . . . C44 C 0.4710(3) 0.8028(3) 0.0935(2) 0.0217(8) Uani 1 1 d . . . . . C45 C 0.5430(3) 0.7878(3) 0.1666(2) 0.0219(8) Uani 1 1 d . . . . . H45 H 0.581055 0.841416 0.193345 0.026 Uiso 1 1 calc R U . . . C46 C 0.5590(3) 0.6951(3) 0.2002(2) 0.0206(8) Uani 1 1 d . . . . . H46 H 0.608120 0.686922 0.248922 0.025 Uiso 1 1 calc R U . . . C47 C 0.4578(4) 0.9035(3) 0.0563(3) 0.0315(10) Uani 1 1 d . . . . . H47A H 0.409620 0.942747 0.080351 0.047 Uiso 1 1 calc R U . . . H47B H 0.426119 0.897226 0.000733 0.047 Uiso 1 1 calc R U . . . H47C H 0.529288 0.934768 0.063988 0.047 Uiso 1 1 calc R 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 Re1 0.01528(10) 0.01709(11) 0.01986(11) 0.00284(7) 0.00306(7) -0.00133(7) Br1A 0.0214(4) 0.0161(4) 0.0230(3) -0.0016(3) 0.0066(2) -0.0012(4) Br1B 0.026(2) 0.029(3) 0.0293(17) 0.006(2) 0.0091(14) 0.003(2) P1 0.0153(5) 0.0136(5) 0.0198(5) -0.0010(4) 0.0047(4) -0.0010(4) O3 0.0416(19) 0.0359(19) 0.0229(17) 0.0038(14) -0.0003(14) -0.0060(15) O1 0.0207(16) 0.049(2) 0.0430(19) 0.0091(17) 0.0063(14) -0.0116(15) O2A 0.038(3) 0.030(5) 0.044(4) 0.008(3) 0.016(2) 0.015(3) N11 0.0160(16) 0.0190(17) 0.0228(17) -0.0015(14) 0.0061(13) -0.0011(13) N12 0.0174(16) 0.0161(16) 0.0202(16) -0.0002(13) 0.0056(13) -0.0021(13) N21 0.0167(16) 0.0190(18) 0.0234(17) -0.0020(13) 0.0031(13) 0.0020(13) N22 0.0150(17) 0.030(2) 0.046(2) -0.0080(17) 0.0056(16) 0.0008(15) C1 0.0196(19) 0.0158(19) 0.0197(19) 0.0000(15) 0.0038(15) 0.0003(16) C2 0.0160(18) 0.0144(18) 0.0202(19) 0.0027(15) 0.0041(15) -0.0001(15) C3 0.0171(19) 0.018(2) 0.026(2) 0.0008(16) 0.0046(16) 0.0006(16) C4 0.022(2) 0.020(2) 0.031(2) -0.0039(17) 0.0038(17) -0.0061(17) C5 0.029(2) 0.024(2) 0.024(2) -0.0062(17) 0.0079(17) -0.0018(18) C6 0.022(2) 0.019(2) 0.025(2) -0.0009(16) 0.0081(16) 0.0001(16) C7 0.0159(19) 0.0133(19) 0.025(2) 0.0016(15) 0.0061(15) -0.0006(15) C10 0.023(2) 0.020(2) 0.026(2) 0.0028(17) 0.0045(18) -0.0019(16) C8 0.023(2) 0.027(2) 0.021(2) 0.0025(17) 0.0002(16) -0.0010(18) C9A 0.025(4) 0.023(5) 0.029(4) 0.010(3) 0.005(3) -0.005(4) C11 0.019(2) 0.027(2) 0.032(2) 0.0010(18) 0.0097(17) -0.0046(17) C12 0.027(2) 0.032(2) 0.032(2) 0.007(2) 0.0101(18) -0.0046(19) C13 0.026(2) 0.026(2) 0.026(2) 0.0058(18) 0.0064(17) -0.0027(18) C21 0.026(2) 0.021(2) 0.047(3) -0.003(2) 0.007(2) 0.0031(18) C22 0.029(2) 0.027(3) 0.058(3) -0.013(2) 0.004(2) 0.009(2) C23 0.019(2) 0.036(3) 0.036(3) -0.004(2) 0.0060(18) 0.0059(19) C31 0.0144(18) 0.017(2) 0.024(2) 0.0006(15) 0.0046(15) 0.0000(15) C32 0.021(2) 0.018(2) 0.030(2) 0.0028(17) 0.0060(17) 0.0020(16) C33 0.019(2) 0.020(2) 0.032(2) 0.0038(17) 0.0077(17) -0.0022(16) C34 0.0168(19) 0.022(2) 0.0187(19) -0.0007(16) 0.0016(15) -0.0005(16) C35 0.023(2) 0.019(2) 0.022(2) 0.0017(16) 0.0065(16) 0.0026(16) C36 0.025(2) 0.017(2) 0.026(2) 0.0036(16) 0.0087(17) 0.0025(17) C37 0.026(2) 0.022(2) 0.029(2) 0.0026(17) 0.0116(17) 0.0019(17) C41 0.0174(18) 0.0155(19) 0.0224(19) 0.0009(15) 0.0100(15) 0.0015(15) C42 0.0192(19) 0.018(2) 0.022(2) -0.0004(16) 0.0057(15) -0.0001(16) C43 0.021(2) 0.024(2) 0.0197(19) 0.0036(16) 0.0061(15) 0.0045(17) C44 0.023(2) 0.020(2) 0.026(2) 0.0010(17) 0.0130(16) 0.0022(17) C45 0.022(2) 0.016(2) 0.028(2) -0.0014(16) 0.0064(16) -0.0018(16) C46 0.0197(19) 0.020(2) 0.022(2) 0.0030(16) 0.0042(15) 0.0000(16) C47 0.031(2) 0.027(2) 0.035(2) 0.011(2) 0.0061(19) 0.0030(19) 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' 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4 -5 -6 0.0813 4 5 6 0.0383 -7 3 6 0.1387 7 -3 -6 0.1387 6 1 -9 0.1000 -6 -1 9 0.1000 -7 1 -4 0.0906 7 -1 4 0.0906 2 7 -7 0.0962 0 -6 8 0.1269 -4 8 1 0.1438 4 -8 -1 0.1838 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 Br1B Re1 Br1A 166.97(11) . . ? P1 Re1 Br1A 93.22(3) . . ? P1 Re1 Br1B 96.00(11) . . ? N12 Re1 Br1A 85.60(9) . . ? N12 Re1 Br1B 84.48(13) . . ? N12 Re1 P1 94.78(9) . . ? C10 Re1 Br1A 86.50(12) . . ? C10 Re1 Br1B 85.08(16) . . ? C10 Re1 P1 175.18(12) . . ? C10 Re1 N12 90.00(15) . . ? C10 Re1 C9B 85.1(8) . . ? C8 Re1 Br1A 94.95(13) . . ? C8 Re1 Br1B 94.75(16) . . ? C8 Re1 P1 86.72(12) . . ? C8 Re1 N12 178.37(15) . . ? C8 Re1 C10 88.50(17) . . ? C8 Re1 C9B 92.4(8) . . ? C9A Re1 Br1A 172.3(2) . . ? C9A Re1 Br1B 5.9(3) . . ? C9A Re1 P1 90.7(2) . . ? C9A Re1 N12 87.5(3) . . ? C9A Re1 C10 90.2(3) . . ? C9A Re1 C8 91.9(3) . . ? C9A Re1 C9B 173.5(8) . . ? C9B Re1 Br1A 2.8(8) . . ? C9B Re1 Br1B 167.7(8) . . ? C9B Re1 P1 94.4(8) . . ? C9B Re1 N12 88.1(8) . . ? C9B Br1A Re1 10(3) . . ? O2A Br1B Re1 161.5(14) . . ? O2A Br1B C9A 144.3(19) . . ? C9A Br1B Re1 17.2(9) . . ? C1 P1 Re1 116.41(13) . . ? C31 P1 Re1 112.56(13) . . ? C31 P1 C1 104.71(18) . . ? C41 P1 Re1 116.74(13) . . ? C41 P1 C1 103.51(18) . . ? C41 P1 C31 101.10(18) . . ? Br1B O2A C9A 19.2(11) . . ? N12 N11 C7 120.1(3) . . ? C11 N11 N12 111.2(3) . . ? C11 N11 C7 127.8(3) . . ? N11 N12 Re1 129.9(2) . . ? C13 N12 Re1 125.3(3) . . ? C13 N12 N11 104.7(3) . . ? N22 N21 C7 122.7(3) . . ? C21 N21 N22 111.7(3) . . ? C21 N21 C7 125.3(4) . . ? C23 N22 N21 103.6(4) . . ? C2 C1 P1 120.8(3) . . ? C6 C1 P1 120.4(3) . . ? C6 C1 C2 118.8(4) . . ? C1 C2 C7 119.1(3) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C7 121.2(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.6 . . ? C3 C4 H4 119.9 . . ? C3 C4 C5 120.3(4) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 120.3 . . ? C4 C5 C6 119.5(4) . . ? C6 C5 H5 120.3 . . ? C1 C6 H6 119.4 . . ? C5 C6 C1 121.1(4) . . ? C5 C6 H6 119.4 . . ? N11 C7 C2 109.3(3) . . ? N11 C7 H7 106.7 . . ? N21 C7 N11 109.9(3) . . ? N21 C7 C2 117.0(3) . . ? N21 C7 H7 106.7 . . ? C2 C7 H7 106.7 . . ? O3 C10 Re1 175.1(4) . . ? O1 C8 Re1 178.7(4) . . ? Br1B C9A Re1 156.9(12) . . ? Br1B C9A O2A 16.5(9) . . ? O2A C9A Re1 173.4(8) . . ? Br1A C9B Re1 168(3) . . ? Br1A C9B O2B 7.2(14) . . ? O2B C9B Re1 173(3) . . ? N11 C11 H11 126.4 . . ? N11 C11 C12 107.2(4) . . ? C12 C11 H11 126.4 . . ? C11 C12 H12 127.4 . . ? C11 C12 C13 105.1(4) . . ? C13 C12 H12 127.4 . . ? N12 C13 C12 111.8(4) . . ? N12 C13 H13 124.1 . . ? C12 C13 H13 124.1 . . ? N21 C21 H21 126.5 . . ? N21 C21 C22 107.1(4) . . ? C22 C21 H21 126.5 . . ? C21 C22 H22 127.5 . . ? C21 C22 C23 105.1(4) . . ? C23 C22 H22 127.5 . . ? N22 C23 C22 112.5(4) . . ? N22 C23 H23 123.7 . . ? C22 C23 H23 123.7 . . ? C32 C31 P1 121.4(3) . . ? C32 C31 C36 117.8(4) . . ? C36 C31 P1 120.8(3) . . ? C31 C32 H32 119.2 . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32 119.2 . . ? C32 C33 H33 119.6 . . ? C32 C33 C34 120.9(4) . . ? C34 C33 H33 119.6 . . ? C33 C34 C37 120.0(4) . . ? C35 C34 C33 117.5(4) . . ? C35 C34 C37 122.5(4) . . ? C34 C35 H35 119.0 . . ? C36 C35 C34 121.9(4) . . ? C36 C35 H35 119.0 . . ? C31 C36 H36 119.8 . . ? C35 C36 C31 120.5(4) . . ? C35 C36 H36 119.8 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C42 C41 P1 121.6(3) . . ? C42 C41 C46 118.8(4) . . ? C46 C41 P1 119.0(3) . . ? C41 C42 H42 120.0 . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 120.0 . . ? C42 C43 H43 119.2 . . ? C42 C43 C44 121.6(4) . . ? C44 C43 H43 119.2 . . ? C43 C44 C47 121.7(4) . . ? C45 C44 C43 117.6(4) . . ? C45 C44 C47 120.7(4) . . ? C44 C45 H45 119.3 . . ? C46 C45 C44 121.3(4) . . ? C46 C45 H45 119.3 . . ? C41 C46 H46 119.7 . . ? C45 C46 C41 120.5(4) . . ? C45 C46 H46 119.7 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? 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 Re1 Br1A 2.6057(11) . ? Re1 Br1B 2.531(5) . ? Re1 P1 2.4892(10) . ? Re1 N12 2.209(3) . ? Re1 C10 1.976(4) . ? Re1 C8 1.925(4) . ? Re1 C9A 1.907(9) . ? Re1 C9B 2.02(3) . ? Br1A C9B 0.60(3) . ? Br1B O2A 0.575(5) . ? Br1B C9A 0.664(6) . ? P1 C1 1.842(4) . ? P1 C31 1.837(4) . ? P1 C41 1.830(4) . ? O3 C10 1.127(5) . ? O1 C8 1.145(5) . ? O2A C9A 1.179(10) . ? O2B C9B 1.06(3) . ? N11 N12 1.367(4) . ? N11 C7 1.477(5) . ? N11 C11 1.340(5) . ? N12 C13 1.329(5) . ? N21 N22 1.367(5) . ? N21 C7 1.444(5) . ? N21 C21 1.352(5) . ? N22 C23 1.327(6) . ? C1 C2 1.411(5) . ? C1 C6 1.398(6) . ? C2 C3 1.389(5) . ? C2 C7 1.516(6) . ? C3 H3 0.9300 . ? C3 C4 1.385(6) . ? C4 H4 0.9300 . ? C4 C5 1.386(6) . ? C5 H5 0.9300 . ? C5 C6 1.389(6) . ? C6 H6 0.9300 . ? C7 H7 0.9800 . ? C11 H11 0.9300 . ? C11 C12 1.377(6) . ? C12 H12 0.9300 . ? C12 C13 1.379(6) . ? C13 H13 0.9300 . ? C21 H21 0.9300 . ? C21 C22 1.359(6) . ? C22 H22 0.9300 . ? C22 C23 1.386(7) . ? C23 H23 0.9300 . ? C31 C32 1.392(6) . ? C31 C36 1.399(5) . ? C32 H32 0.9300 . ? C32 C33 1.377(6) . ? C33 H33 0.9300 . ? C33 C34 1.401(6) . ? C34 C35 1.387(6) . ? C34 C37 1.498(6) . ? C35 H35 0.9300 . ? C35 C36 1.379(6) . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C41 C42 1.389(5) . ? C41 C46 1.399(5) . ? C42 H42 0.9300 . ? C42 C43 1.384(6) . ? C43 H43 0.9300 . ? C43 C44 1.398(6) . ? C44 C45 1.391(6) . ? C44 C47 1.502(6) . ? C45 H45 0.9300 . ? C45 C46 1.379(6) . ? C46 H46 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? 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 Re1 Br1A C9B O2B 148(15) . . . . ? Re1 Br1B O2A C9A 1(2) . . . . ? Re1 Br1B C9A O2A -179(3) . . . . ? Re1 P1 C1 C2 51.4(4) . . . . ? Re1 P1 C1 C6 -127.3(3) . . . . ? Re1 P1 C31 C32 -116.3(3) . . . . ? Re1 P1 C31 C36 60.2(3) . . . . ? Re1 P1 C41 C42 -152.8(3) . . . . ? Re1 P1 C41 C46 36.1(4) . . . . ? Re1 N12 C13 C12 177.8(3) . . . . ? P1 C1 C2 C3 -177.0(3) . . . . ? P1 C1 C2 C7 -1.3(5) . . . . ? P1 C1 C6 C5 176.8(3) . . . . ? P1 C31 C32 C33 177.2(3) . . . . ? P1 C31 C36 C35 -177.5(3) . . . . ? P1 C41 C42 C43 -169.9(3) . . . . ? P1 C41 C46 C45 170.6(3) . . . . ? O2A Br1B C9A Re1 179(3) . . . . ? N11 N12 C13 C12 0.8(5) . . . . ? N11 C11 C12 C13 -1.5(5) . . . . ? N12 N11 C7 N21 -145.8(3) . . . . ? N12 N11 C7 C2 84.6(4) . . . . ? N12 N11 C11 C12 2.1(5) . . . . ? N21 N22 C23 C22 -0.7(6) . . . . ? N21 C21 C22 C23 0.4(6) . . . . ? N22 N21 C7 N11 -69.3(5) . . . . ? N22 N21 C7 C2 56.0(5) . . . . ? N22 N21 C21 C22 -0.9(6) . . . . ? C1 P1 C31 C32 116.3(3) . . . . ? C1 P1 C31 C36 -67.1(4) . . . . ? C1 P1 C41 C42 -23.5(4) . . . . ? C1 P1 C41 C46 165.4(3) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C1 C2 C7 N11 -95.8(4) . . . . ? C1 C2 C7 N21 138.5(4) . . . . ? C2 C1 C6 C5 -2.0(6) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C2 C7 N11 79.8(4) . . . . ? C3 C2 C7 N21 -45.8(5) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C4 C5 C6 C1 1.0(6) . . . . ? C6 C1 C2 C3 1.7(6) . . . . ? C6 C1 C2 C7 177.4(3) . . . . ? C7 N11 N12 Re1 11.8(5) . . . . ? C7 N11 N12 C13 -171.5(3) . . . . ? C7 N11 C11 C12 170.8(4) . . . . ? C7 N21 N22 C23 174.3(4) . . . . ? C7 N21 C21 C22 -174.0(4) . . . . ? C7 C2 C3 C4 -176.2(4) . . . . ? C11 N11 N12 Re1 -178.5(3) . . . . ? C11 N11 N12 C13 -1.8(4) . . . . ? C11 N11 C7 N21 46.4(5) . . . . ? C11 N11 C7 C2 -83.2(5) . . . . ? C11 C12 C13 N12 0.4(5) . . . . ? C21 N21 N22 C23 0.9(5) . . . . ? C21 N21 C7 N11 103.1(5) . . . . ? C21 N21 C7 C2 -131.6(4) . . . . ? C21 C22 C23 N22 0.2(6) . . . . ? C31 P1 C1 C2 176.4(3) . . . . ? C31 P1 C1 C6 -2.3(4) . . . . ? C31 P1 C41 C42 84.8(3) . . . . ? C31 P1 C41 C46 -86.4(3) . . . . ? C31 C32 C33 C34 -0.2(6) . . . . ? C32 C31 C36 C35 -0.8(6) . . . . ? C32 C33 C34 C35 0.1(6) . . . . ? C32 C33 C34 C37 -179.2(4) . . . . ? C33 C34 C35 C36 -0.5(6) . . . . ? C34 C35 C36 C31 0.8(6) . . . . ? C36 C31 C32 C33 0.5(6) . . . . ? C37 C34 C35 C36 178.8(4) . . . . ? C41 P1 C1 C2 -78.1(3) . . . . ? C41 P1 C1 C6 103.2(3) . . . . ? C41 P1 C31 C32 9.0(4) . . . . ? C41 P1 C31 C36 -174.5(3) . . . . ? C41 C42 C43 C44 -0.3(6) . . . . ? C42 C41 C46 C45 -0.8(6) . . . . ? C42 C43 C44 C45 -1.2(6) . . . . ? C42 C43 C44 C47 178.1(4) . . . . ? C43 C44 C45 C46 1.6(6) . . . . ? C44 C45 C46 C41 -0.7(6) . . . . ? C46 C41 C42 C43 1.3(6) . . . . ? C47 C44 C45 C46 -177.6(4) . . . . ? 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 -4.0032 -5.0066 -5.9927 0.9893 0.1736 0.0484 4.0032 5.0066 5.9927 -0.9893 -0.1736 -0.0484 -7.0012 3.0013 6.0063 0.0628 0.0003 -0.9984 7.0012 -3.0013 -6.0063 -0.0628 -0.0003 0.9984 5.9990 0.9976 -9.0085 -0.1449 0.5288 0.8332 -5.9990 -0.9976 9.0085 0.1449 -0.5288 -0.8332 -7.0047 0.9950 -3.9935 0.6839 0.5556 -0.5656 7.0047 -0.9950 3.9935 -0.6839 -0.5556 0.5656 1.9970 6.9987 -7.0082 -0.3685 0.9398 0.1249 0.0041 -5.9970 8.0054 0.0818 -0.9953 -0.0145 -4.0027 8.0011 0.9987 -0.3290 0.6260 -0.7610 4.0027 -8.0011 -0.9987 0.3290 -0.6260 0.7610