#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:38:48 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132567.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_4132567 loop_ _publ_author_name 'Yuan, Shuai' 'Zhang, Peng' 'Zhang, Liangliang' 'Garcia-Esparza, Angel T' 'Sokaras, Dimosthenis' 'Qin, Jun-Sheng' 'Feng, Liang' 'Day, Gregory S.' 'Chen, Wenmiao' 'Drake, Hannah F.' 'Elumalai, Palani' 'Madrahimov, Sherzod T.' 'Sun, Daofeng' 'Zhou, Hong-Cai' _publ_section_title ; Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10814 _journal_page_last 10819 _journal_paper_doi 10.1021/jacs.8b04886 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C12 H16 N2 Ni O8' _chemical_formula_sum 'C12 H16 N2 Ni O8' _chemical_formula_weight 374.98 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-05-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _cell_angle_alpha 96.319(2) _cell_angle_beta 105.067(2) _cell_angle_gamma 113.408(2) _cell_formula_units_Z 1 _cell_length_a 6.2763(4) _cell_length_b 6.8351(4) _cell_length_c 9.2430(6) _cell_measurement_reflns_used 4879 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.556 _cell_measurement_theta_min 2.351 _cell_volume 341.04(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6949 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.556 _diffrn_reflns_theta_min 2.351 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6890 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour greenish _exptl_crystal_colour_modifier greenish _exptl_crystal_density_diffrn 1.826 _exptl_crystal_description needle _exptl_crystal_F_000 194 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.836 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.103 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 108 _refine_ls_number_reflns 1582 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.127 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0401 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.7105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.0875 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1440 _reflns_number_total 1582 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04886_si_002.cif _cod_data_source_block NiINA2O _cod_database_code 4132567 _shelx_shelxl_version_number 2014/7 _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 0.943 _shelx_estimated_absorpt_t_min 0.867 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2.a Rotating group: O3(H3a,H3b) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4a), C6(H6), C5(H5) 2.c Tetrahedral OH refined with riding coordinates: O1(H1) 2.d Idealised tetrahedral OH refined as rotating group: O4(H4) ; _shelx_res_file ; NiINA2O.res created by SHELXL-2014/7 TITL NiINA2O_a.res in P-1 REM Old TITL NiINA2O in P-1 #2 REM SHELXT solution in P-1 REM R1 0.059, Rweak 0.021, Alpha 0.034, Orientation as input REM Formula found by SHELXT: C12 N2 Ni O8 CELL 0.71073 6.2763 6.8351 9.243 96.319 105.067 113.408 ZERR 1 0.0004 0.0004 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H N Ni O UNIT 12 16 2 1 8 L.S. 99 PLAN 10 SIZE 0.04 0.04 0.1 BOND $H list 4 fmap 2 acta 52 REM REM REM WGHT 0.029100 0.710500 FVAR 1.15682 NI1 4 1.000000 0.500000 1.000000 10.50000 0.00840 0.01195 = 0.00728 0.00171 0.00197 0.00497 O2 5 0.077664 0.083852 0.262955 11.00000 0.01187 0.01641 = 0.01343 0.00248 0.00170 0.00528 O3 5 1.221449 0.763684 0.927554 11.00000 0.01176 0.01724 = 0.01349 0.00554 0.00527 0.00755 AFIX 7 H3A 2 1.131539 0.808003 0.863142 11.00000 -1.50000 H3B 2 1.296712 0.721975 0.872295 11.00000 -1.50000 AFIX 0 O4 5 0.820419 0.684780 1.041847 11.00000 0.01114 0.01301 = 0.01083 -0.00079 0.00188 0.00507 AFIX 147 H4 2 0.920619 0.803790 1.100890 11.00000 -1.50000 AFIX 0 O1 5 0.422289 0.230134 0.202234 11.00000 0.01589 0.02543 = 0.00968 0.00521 0.00329 0.01156 AFIX 83 H1 2 0.323787 0.193803 0.114685 11.00000 -1.50000 AFIX 0 N1 3 0.761873 0.360760 0.772563 11.00000 0.01343 0.01033 = 0.00966 0.00213 0.00359 0.00635 C3 1 0.716578 0.295356 0.503795 11.00000 0.01337 0.01227 = 0.01195 0.00361 0.00624 0.00576 AFIX 43 H3 2 0.789398 0.296156 0.428009 11.00000 -1.20000 AFIX 0 C1 1 0.307396 0.174575 0.295167 11.00000 0.01524 0.01023 = 0.01374 0.00284 0.00426 0.00857 C4 1 0.856521 0.358511 0.657478 11.00000 0.01105 0.01290 = 0.01276 0.00274 0.00479 0.00555 AFIX 43 H4A 2 1.024782 0.401811 0.683291 11.00000 -1.20000 AFIX 0 C6 1 0.363802 0.222248 0.580990 11.00000 0.01052 0.01149 = 0.01322 0.00106 0.00247 0.00629 AFIX 43 H6 2 0.194883 0.172386 0.557872 11.00000 -1.20000 AFIX 0 C5 1 0.516838 0.288996 0.732356 11.00000 0.01162 0.01529 = 0.01438 0.00250 0.00625 0.00741 AFIX 43 H5 2 0.447415 0.284158 0.810166 11.00000 -1.20000 AFIX 0 C2 1 0.464933 0.230332 0.463241 11.00000 0.01139 0.00687 = 0.01302 0.00354 0.00354 0.00563 HKLF 4 REM NiINA2O_a.res in P-1 REM R1 = 0.0401 for 1440 Fo > 4sig(Fo) and 0.0487 for all 1582 data REM 108 parameters refined using 0 restraints END WGHT 0.0291 0.7105 REM Highest difference peak 0.836, deepest hole -0.823, 1-sigma level 0.103 Q1 1 0.7219 0.7028 0.9579 11.00000 0.05 0.84 Q2 1 1.3655 0.8099 0.9064 11.00000 0.05 0.50 Q3 1 0.8456 0.4009 0.8575 11.00000 0.05 0.48 Q4 1 0.4116 0.1999 0.5205 11.00000 0.05 0.39 Q5 1 0.4005 0.2191 0.3972 11.00000 0.05 0.38 Q6 1 0.7806 0.2631 0.5754 11.00000 0.05 0.35 Q7 1 0.1765 0.1037 0.6208 11.00000 0.05 0.33 Q8 1 0.1657 0.2472 0.4774 11.00000 0.05 0.32 Q9 1 0.8012 0.3606 0.7260 11.00000 0.05 0.31 Q10 1 0.8461 0.6047 1.0148 11.00000 0.05 0.31 ; _shelx_res_checksum 10333 _shelx_hkl_file ; -1 0 0 208.39 6.73 -1 0 0 201.82 7.51 -1 0 0 195.51 6.45 1 0 0 187.56 7.18 1 0 0 201.53 5.91 1 0 0 191.42 7.35 1 0 0 201.03 6.53 1 0 0 207.17 6.83 -2 0 0 51.11 4.78 -2 0 0 45.83 4.38 -2 0 0 50.81 6.31 2 0 0 39.33 4.71 2 0 0 48.88 4.71 2 0 0 39.00 5.56 2 0 0 46.88 5.20 2 0 0 44.55 4.22 -3 0 0 5.05 3.08 3 0 0 11.34 3.86 3 0 0 4.21 3.02 3 0 0 2.43 4.27 3 0 0 7.13 4.19 3 0 0 6.03 4.47 3 0 0 2.90 3.84 3 0 0 6.79 3.52 -4 0 0 541.18 20.99 4 0 0 527.21 23.44 4 0 0 529.03 22.06 4 0 0 522.04 20.97 4 0 0 529.23 20.41 4 0 0 533.20 18.87 4 0 0 535.61 23.89 4 0 0 515.34 25.25 -5 0 0 248.86 16.48 5 0 0 196.24 15.68 5 0 0 216.37 19.40 5 0 0 243.15 20.64 5 0 0 182.75 16.76 -6 0 0 106.96 17.84 6 0 0 129.68 21.55 6 0 0 129.74 20.96 6 0 0 158.05 24.86 7 0 0 24.64 21.31 7 0 0 -11.21 22.21 7 -1 0 76.85 19.04 7 -1 0 47.26 21.91 7 -1 0 42.50 20.15 6 -1 0 313.09 25.20 6 -1 0 287.72 28.50 6 -1 0 238.03 21.46 6 -1 0 276.10 26.55 -6 1 0 248.13 18.07 5 -1 0 655.79 30.04 5 -1 0 614.73 24.09 5 -1 0 631.13 24.06 5 -1 0 699.93 30.60 -5 1 0 660.18 26.32 -5 1 0 677.92 24.04 4 -1 0 654.66 23.47 4 -1 0 720.35 25.01 4 -1 0 738.02 27.86 4 -1 0 729.63 27.42 4 -1 0 744.18 23.47 4 -1 0 688.88 22.29 -4 1 0 695.14 23.88 -4 1 0 678.80 21.63 3 -1 0 727.74 19.05 3 -1 0 754.04 21.59 3 -1 0 717.95 21.66 3 -1 0 722.61 24.78 3 -1 0 719.07 24.51 -3 1 0 721.21 19.12 -3 1 0 710.16 21.45 -3 1 0 713.60 26.00 2 -1 0 1001.99 25.86 2 -1 0 1033.75 22.96 2 -1 0 1026.13 26.68 2 -1 0 1018.65 19.61 -2 1 0 1021.84 27.19 -2 1 0 974.78 19.33 -2 1 0 1001.51 22.48 1 -1 0 740.17 15.57 1 -1 0 706.82 17.34 1 -1 0 762.02 15.24 -1 1 0 749.41 18.05 0 -1 0 1104.99 19.90 0 -1 0 1105.41 20.37 0 1 0 1111.78 20.45 0 1 0 1082.64 19.64 0 1 0 1099.82 19.85 -1 -1 0 664.11 17.35 -1 -1 0 659.72 18.33 -1 -1 0 663.37 13.71 -1 -1 0 668.90 14.69 1 1 0 675.61 13.76 1 1 0 649.77 17.67 1 1 0 643.41 13.61 1 1 0 652.28 17.21 -2 -1 0 37.35 3.71 -2 -1 0 29.29 5.18 -2 -1 0 42.86 6.34 2 1 0 35.31 6.43 2 1 0 47.56 5.74 2 1 0 36.24 5.11 2 1 0 40.67 4.39 -3 -1 0 1383.88 36.81 3 1 0 1356.33 36.63 3 1 0 1466.80 34.78 3 1 0 1452.57 32.08 3 1 0 1395.89 35.79 3 1 0 1389.60 30.04 3 1 0 1431.43 37.05 3 1 0 1422.77 39.79 -4 -1 0 392.27 20.33 4 1 0 383.98 20.69 4 1 0 376.80 22.90 4 1 0 357.28 15.67 4 1 0 381.09 19.21 4 1 0 353.82 19.76 4 1 0 369.03 17.18 -5 -1 0 140.43 17.60 5 1 0 187.50 15.57 5 1 0 169.72 21.16 5 1 0 146.09 18.89 5 1 0 165.25 21.89 5 1 0 124.50 18.27 -6 -1 0 184.45 24.29 6 1 0 143.01 26.39 6 1 0 209.61 31.16 7 -2 0 56.75 17.29 7 -2 0 76.28 19.41 6 -2 0 12.23 11.60 6 -2 0 11.47 12.43 6 -2 0 29.39 9.82 -6 2 0 5.87 8.42 -6 2 0 20.64 7.24 5 -2 0 267.02 21.42 5 -2 0 256.55 13.93 5 -2 0 282.32 20.38 -5 2 0 278.81 16.89 -5 2 0 259.93 12.80 4 -2 0 444.35 14.50 4 -2 0 436.34 21.65 4 -2 0 449.30 22.30 4 -2 0 442.88 19.08 4 -2 0 409.96 17.78 -4 2 0 434.59 18.07 -4 2 0 435.56 23.99 -4 2 0 438.81 14.02 3 -2 0 2076.30 43.28 3 -2 0 2088.25 49.26 3 -2 0 2040.22 34.84 3 -2 0 2031.44 48.24 3 -2 0 2106.85 43.12 -3 2 0 2076.39 42.63 -3 2 0 2106.94 51.22 -3 2 0 2039.98 34.67 2 -2 0 1554.87 31.32 2 -2 0 1579.52 36.47 2 -2 0 1608.44 32.65 2 -2 0 1526.29 35.90 -2 2 0 1634.02 38.83 -2 2 0 1541.11 32.19 1 -2 0 9729.81 140.29 1 -2 0 9948.62 147.43 1 -2 0 9999.00 144.31 -1 2 0 9998.66 144.75 -1 2 0 9808.03 147.73 -1 2 0 9648.72 138.28 -1 2 0 9931.95 141.00 0 -2 0 2968.37 51.20 0 -2 0 2888.76 49.21 0 -2 0 2936.94 50.00 0 2 0 2911.44 49.80 0 2 0 2932.56 49.96 0 2 0 2939.64 50.98 -1 -2 0 859.55 24.47 -1 -2 0 817.92 18.55 -1 -2 0 871.34 23.85 1 2 0 869.30 24.23 1 2 0 868.26 19.70 -2 -2 0 1017.55 29.82 -2 -2 0 999.22 31.83 -2 -2 0 988.57 22.26 2 2 0 1003.59 22.61 2 2 0 1004.42 30.17 2 2 0 959.18 24.32 -3 -2 0 489.09 22.22 3 2 0 480.89 22.52 3 2 0 457.06 21.63 3 2 0 468.29 15.70 3 2 0 480.10 16.07 3 2 0 432.63 20.24 3 2 0 511.79 17.50 -4 -2 0 0.38 6.94 4 2 0 3.62 5.89 4 2 0 5.82 8.82 4 2 0 2.12 7.32 4 2 0 -5.73 9.47 4 2 0 4.99 6.71 -5 -2 0 -2.26 11.06 5 2 0 7.34 13.87 5 2 0 33.03 11.92 5 2 0 37.59 13.35 6 2 0 99.77 20.77 7 -3 0 155.29 26.15 7 -3 0 108.43 18.30 7 -3 0 166.87 28.71 -7 3 0 107.56 19.15 6 -3 0 44.49 7.98 6 -3 0 57.67 12.84 6 -3 0 62.68 16.43 -6 3 0 83.75 14.39 5 -3 0 67.25 12.11 5 -3 0 81.21 14.63 5 -3 0 66.91 7.57 -5 3 0 48.80 6.48 -5 3 0 63.38 13.92 -5 3 0 63.59 10.88 4 -3 0 8.45 5.54 4 -3 0 17.27 5.72 4 -3 0 18.10 6.80 4 -3 0 20.52 7.11 -4 3 0 16.33 4.60 -4 3 0 25.08 9.24 3 -3 0 2850.43 54.67 3 -3 0 2865.91 62.61 3 -3 0 2774.62 55.53 3 -3 0 2916.94 62.99 -3 3 0 2842.85 65.34 -3 3 0 2897.78 56.40 2 -3 0 198.27 12.82 2 -3 0 199.73 11.61 2 -3 0 214.07 11.09 -2 3 0 187.47 13.27 -2 3 0 195.82 10.71 -2 3 0 189.04 6.31 1 -3 0 169.54 9.95 1 -3 0 156.94 6.78 1 -3 0 144.32 9.58 -1 3 0 151.54 9.18 -1 3 0 154.72 10.84 -1 3 0 146.12 7.05 0 -3 0 83.01 8.02 0 -3 0 88.01 7.20 0 -3 0 83.53 6.77 0 3 0 82.35 7.58 0 3 0 98.90 7.95 0 3 0 79.37 6.66 -1 -3 0 95.93 10.32 -1 -3 0 100.94 9.18 -1 -3 0 94.68 6.66 1 3 0 89.56 8.22 1 3 0 98.73 9.08 1 3 0 101.64 9.90 -2 -3 0 1387.72 39.37 -2 -3 0 1365.74 29.64 -2 -3 0 1354.08 41.71 2 3 0 1364.26 31.12 2 3 0 1426.79 40.12 2 3 0 1372.12 39.35 -3 -3 0 383.90 13.96 3 3 0 415.06 23.56 3 3 0 367.92 24.44 3 3 0 367.61 14.27 -4 -3 0 281.68 22.35 4 3 0 242.96 23.29 4 3 0 268.12 23.57 4 3 0 276.99 15.97 -5 -3 0 199.03 26.97 5 3 0 192.05 28.12 7 -4 0 102.30 19.55 7 -4 0 73.35 20.24 -7 4 0 74.39 13.92 6 -4 0 542.96 32.27 6 -4 0 489.92 30.47 -6 4 0 521.78 26.08 5 -4 0 339.12 23.52 5 -4 0 317.52 22.85 -5 4 0 313.64 18.93 4 -4 0 382.52 22.29 4 -4 0 351.09 18.83 4 -4 0 367.89 21.64 4 -4 0 369.29 17.95 -4 4 0 386.08 25.78 -4 4 0 368.02 18.36 3 -4 0 352.71 18.84 3 -4 0 351.04 19.74 3 -4 0 343.27 16.36 3 -4 0 367.60 15.25 -3 4 0 360.18 16.98 -3 4 0 352.79 21.37 2 -4 0 2914.68 53.06 2 -4 0 3071.91 60.27 2 -4 0 2939.84 58.92 2 -4 0 2947.09 63.34 -2 4 0 2970.93 60.02 -2 4 0 2899.11 49.17 -2 4 0 2988.55 65.93 1 -4 0 120.41 10.00 1 -4 0 108.09 10.59 1 -4 0 123.58 6.26 -1 4 0 109.20 9.66 -1 4 0 135.74 12.74 -1 4 0 112.21 8.20 0 -4 0 885.29 29.29 0 -4 0 894.56 25.94 0 -4 0 900.52 27.57 0 4 0 858.47 28.00 0 4 0 882.86 26.67 0 4 0 886.90 28.21 -1 -4 0 10.48 5.36 -1 -4 0 16.19 7.22 -1 -4 0 18.26 4.28 1 4 0 7.89 6.28 1 4 0 16.39 5.97 1 4 0 4.73 5.83 -2 -4 0 25.58 7.63 -2 -4 0 21.53 5.02 2 4 0 17.05 7.43 2 4 0 28.62 9.07 -3 -4 0 78.72 13.52 -3 -4 0 100.13 10.01 -4 -4 0 237.59 26.75 4 4 0 217.27 29.50 7 -5 0 144.20 27.97 7 -5 0 163.05 30.18 -7 5 0 165.32 22.05 6 -5 0 271.63 26.49 6 -5 0 269.91 26.14 -6 5 0 334.52 22.16 5 -5 0 6.36 8.58 -5 5 0 24.19 8.20 4 -5 0 488.18 25.34 4 -5 0 491.51 26.75 4 -5 0 490.78 21.42 -4 5 0 525.12 23.34 3 -5 0 23.34 8.55 3 -5 0 44.93 8.44 3 -5 0 34.73 8.87 3 -5 0 40.76 6.78 -3 5 0 23.36 5.80 -3 5 0 37.65 9.57 2 -5 0 498.07 23.31 2 -5 0 462.57 21.37 2 -5 0 501.43 19.47 2 -5 0 478.32 16.28 -2 5 0 452.80 25.52 -2 5 0 471.13 21.37 -2 5 0 490.18 16.16 -2 5 0 455.89 18.92 1 -5 0 519.70 22.59 1 -5 0 508.73 23.31 -1 5 0 523.09 19.59 -1 5 0 543.03 23.21 -1 5 0 525.70 24.61 -1 5 0 510.58 25.38 0 -5 0 276.26 15.16 0 -5 0 290.71 17.09 0 5 0 256.80 16.29 0 5 0 272.07 19.42 0 5 0 309.95 18.82 -1 -5 0 503.72 19.39 -1 -5 0 536.47 26.15 1 5 0 528.07 24.94 1 5 0 515.25 25.92 -2 -5 0 139.75 11.94 -2 -5 0 148.48 19.02 2 5 0 157.05 19.65 3 5 0 227.19 25.83 7 -6 0 332.24 37.00 7 -6 0 420.48 37.04 -7 6 0 383.02 27.88 6 -6 0 213.64 24.26 6 -6 0 163.94 26.99 -6 6 0 141.96 20.65 5 -6 0 242.66 23.04 5 -6 0 231.25 24.29 -5 6 0 213.30 18.61 4 -6 0 319.44 24.06 4 -6 0 337.98 22.01 4 -6 0 309.93 21.07 -4 6 0 341.59 21.10 3 -6 0 582.05 29.13 3 -6 0 544.95 23.72 3 -6 0 554.82 20.87 -3 6 0 543.03 16.11 -3 6 0 579.47 18.22 2 -6 0 165.97 12.18 2 -6 0 161.80 10.33 2 -6 0 176.40 15.83 -2 6 0 157.89 11.46 -2 6 0 187.50 15.32 1 -6 0 255.56 17.72 -1 6 0 256.57 21.25 -1 6 0 257.47 19.26 -1 6 0 235.22 23.77 -1 6 0 238.01 15.87 0 6 0 59.46 13.88 0 6 0 99.35 20.45 0 6 0 56.77 11.54 -1 -6 0 226.11 16.32 1 6 0 263.55 22.43 2 6 0 161.51 24.25 7 -7 0 16.96 18.50 7 -7 0 20.08 25.69 6 -7 0 -23.55 15.73 6 -7 0 -8.34 15.42 -6 7 0 10.17 12.38 5 -7 0 459.52 34.44 5 -7 0 463.31 28.84 -5 7 0 442.35 27.16 4 -7 0 63.48 11.83 -4 7 0 47.44 11.01 3 -7 0 443.62 27.17 3 -7 0 426.11 21.32 3 -7 0 407.36 19.53 -3 7 0 400.25 25.35 -3 7 0 408.97 18.99 -3 7 0 397.39 16.38 2 -7 0 51.92 11.17 -2 7 0 56.96 10.54 -2 7 0 38.04 8.72 -2 7 0 57.26 11.26 1 -7 0 66.56 14.18 -1 7 0 30.53 14.74 -1 7 0 49.50 11.37 0 -7 0 421.18 22.52 0 7 0 416.46 34.95 0 7 0 409.18 28.60 1 7 0 196.68 27.63 1 7 0 224.53 37.97 6 -8 0 40.88 17.47 -6 8 0 27.45 15.70 5 -8 0 152.57 24.27 5 -8 0 124.32 21.36 -5 8 0 150.02 23.41 4 -8 0 147.64 20.51 4 -8 0 156.28 24.38 -4 8 0 134.95 22.02 3 -8 0 25.61 13.72 -3 8 0 -9.83 11.22 2 -8 0 214.96 23.66 -2 8 0 261.32 26.46 -2 8 0 253.05 26.97 1 -8 0 24.81 12.16 -1 8 0 57.99 18.84 -1 8 0 50.24 14.96 0 8 -1 195.18 39.39 -1 8 -1 172.57 25.23 -1 8 -1 194.44 30.64 1 -8 1 162.24 19.45 -2 8 -1 30.78 11.66 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0 -8 79.99 17.96 6 0 -8 74.32 14.89 -6 0 8 71.03 16.75 5 0 -8 12.49 7.98 5 0 -8 36.23 11.59 -5 0 8 8.47 10.86 -5 0 8 27.25 18.91 4 0 -8 766.62 26.39 4 0 -8 821.83 28.89 4 0 -8 802.37 31.13 4 0 -8 843.08 32.05 -4 0 8 844.72 35.32 -4 0 8 789.44 30.19 3 0 -8 250.86 17.41 3 0 -8 252.73 12.71 3 0 -8 218.40 14.35 3 0 -8 221.88 18.07 -3 0 8 251.94 20.46 -3 0 8 210.38 17.42 2 0 -8 423.33 20.75 2 0 -8 399.84 21.41 -2 0 8 419.90 25.87 -2 0 8 386.23 21.01 1 0 -8 135.58 15.13 1 0 -8 142.74 12.89 -1 0 8 135.37 17.13 0 0 -8 88.95 14.21 0 0 -8 102.68 12.68 0 0 8 125.33 16.14 -1 0 -8 585.50 29.67 -1 0 -8 581.60 25.65 1 0 8 642.61 32.84 -2 0 -8 216.29 18.97 -2 0 -8 235.50 22.91 2 0 8 166.51 25.48 -3 0 -8 162.23 22.42 -3 0 -8 131.31 26.34 3 0 8 158.35 30.20 7 -1 -8 450.07 38.98 7 -1 -8 415.05 30.58 -7 1 8 408.02 34.24 6 -1 -8 18.12 15.93 6 -1 -8 4.84 11.13 -6 1 8 9.76 13.00 5 -1 -8 37.86 10.22 5 -1 -8 32.93 10.27 -5 1 8 29.85 14.35 -5 1 8 41.93 10.96 4 -1 -8 196.61 15.17 4 -1 -8 147.34 16.39 4 -1 -8 178.25 17.28 -4 1 8 202.98 14.36 -4 1 8 218.85 20.37 3 -1 -8 701.38 21.34 3 -1 -8 639.22 32.37 3 -1 -8 755.40 29.81 -3 1 8 742.52 33.37 -3 1 8 713.51 21.21 2 -1 -8 149.29 15.30 2 -1 -8 162.22 13.70 2 -1 -8 157.93 8.33 -2 1 8 126.47 20.66 -2 1 8 142.46 9.56 1 -1 -8 410.53 20.05 1 -1 -8 352.80 22.08 -1 1 8 387.54 25.40 0 -1 -8 52.33 11.80 0 -1 -8 48.80 9.20 0 1 8 57.28 12.50 -1 -1 -8 256.72 22.69 -1 -1 -8 239.87 18.85 1 1 8 253.00 26.70 -2 -1 -8 224.64 20.15 -2 -1 -8 204.05 24.27 2 1 8 250.82 29.72 -3 -1 -8 218.76 27.67 -3 -1 -8 157.73 28.73 7 -2 -8 91.95 18.82 -7 2 8 103.44 17.39 6 -2 -8 45.66 11.95 6 -2 -8 33.84 11.66 -6 2 8 44.17 12.09 -6 2 8 25.80 13.00 5 -2 -8 701.48 31.06 -5 2 8 694.66 28.59 -5 2 8 704.31 32.66 4 -2 -8 30.01 9.21 4 -2 -8 35.11 8.56 -4 2 8 58.65 12.23 -4 2 8 40.52 7.86 3 -2 -8 273.58 18.08 3 -2 -8 287.15 20.02 3 -2 -8 311.35 15.10 -3 2 8 290.76 15.84 -3 2 8 270.30 22.70 2 -2 -8 216.93 15.08 2 -2 -8 185.25 11.93 2 -2 -8 200.24 18.19 -2 2 8 189.59 20.33 -2 2 8 193.66 10.67 1 -2 -8 427.16 14.47 1 -2 -8 455.83 20.67 1 -2 -8 431.30 25.66 -1 2 8 425.44 13.94 -1 2 8 380.87 27.60 -1 2 8 443.65 23.42 0 -2 -8 474.81 28.37 0 -2 -8 483.27 21.67 0 2 8 466.79 31.85 0 2 8 443.46 24.58 -1 -2 -8 -1.13 11.96 1 2 8 33.61 13.99 -2 -2 -8 -8.60 14.49 2 2 8 16.72 18.37 7 -3 -8 4.28 14.51 7 -3 -8 23.96 15.55 -7 3 8 7.32 14.98 -7 3 8 -4.47 14.54 6 -3 -8 298.97 25.51 6 -3 -8 330.01 26.04 -6 3 8 254.44 24.39 -6 3 8 252.99 25.12 5 -3 -8 150.00 17.38 5 -3 -8 177.34 20.95 -5 3 8 163.84 21.14 4 -3 -8 22.37 8.72 4 -3 -8 37.24 10.04 4 -3 -8 10.76 9.23 -4 3 8 15.22 10.87 3 -3 -8 166.12 15.12 3 -3 -8 177.35 15.72 3 -3 -8 162.69 18.16 -3 3 8 157.39 20.78 -3 3 8 158.03 14.26 2 -3 -8 779.05 24.68 2 -3 -8 833.97 36.19 2 -3 -8 777.89 27.72 -2 3 8 841.35 38.35 -2 3 8 789.96 25.18 1 -3 -8 371.61 26.19 1 -3 -8 407.81 18.81 -1 3 8 359.88 17.77 -1 3 8 392.68 29.55 -1 3 8 374.28 25.19 0 -3 -8 329.73 18.92 0 -3 -8 409.58 28.04 0 3 8 332.62 30.96 -1 -3 -8 16.46 15.04 1 3 8 44.47 18.43 7 -4 -8 65.95 17.18 7 -4 -8 86.46 19.45 6 -4 -8 574.01 35.56 6 -4 -8 569.14 32.49 -6 4 8 614.81 32.45 -6 4 8 579.04 31.68 5 -4 -8 17.53 12.40 5 -4 -8 13.94 10.46 -5 4 8 19.84 11.19 -5 4 8 4.63 12.17 4 -4 -8 247.95 19.52 4 -4 -8 271.40 24.05 -4 4 8 226.80 24.27 -4 4 8 254.39 20.49 3 -4 -8 103.55 14.55 3 -4 -8 119.98 20.36 -3 4 8 126.79 21.52 -3 4 8 106.20 16.38 2 -4 -8 221.65 16.17 2 -4 -8 211.96 23.63 -2 4 8 220.13 26.19 -2 4 8 241.18 18.70 1 -4 -8 172.00 23.74 -1 4 8 133.29 18.54 -1 4 8 132.85 20.70 0 -4 -8 14.80 15.57 0 4 8 5.58 17.07 6 -5 -8 7.74 15.14 6 -5 -8 27.88 14.52 -6 5 8 -14.02 16.03 -6 5 8 -21.61 15.49 5 -5 -8 84.69 16.88 5 -5 -8 70.62 12.80 4 -5 -8 53.18 10.90 -4 5 8 47.26 14.43 -4 5 8 87.68 15.21 3 -5 -8 677.33 26.06 3 -5 -8 712.25 38.58 -3 5 8 763.79 39.09 -3 5 8 711.50 33.14 2 -5 -8 7.78 15.32 -2 5 8 59.51 16.70 -2 5 8 33.93 13.94 1 -5 -8 45.82 16.04 -1 5 8 -10.79 18.94 1 6 -9 98.13 19.06 -1 -6 9 77.45 17.03 0 6 -9 134.30 23.99 0 -6 9 72.29 20.07 0 -6 9 113.29 17.94 -1 6 -9 184.85 24.93 1 -6 9 206.34 26.80 1 -6 9 129.32 24.47 -2 6 -9 174.74 27.03 2 -6 9 152.51 27.54 3 5 -9 107.49 18.88 3 5 -9 124.12 24.23 -3 -5 9 112.26 19.72 2 5 -9 38.81 12.04 2 5 -9 57.15 14.89 -2 -5 9 81.14 17.63 1 5 -9 334.36 25.44 1 5 -9 274.24 19.35 -1 -5 9 316.35 28.00 -1 -5 9 267.09 28.81 0 5 -9 -7.34 10.78 0 5 -9 5.30 8.51 0 -5 9 4.51 11.51 0 -5 9 16.21 16.92 -1 5 -9 -2.26 10.88 1 -5 9 3.53 12.36 1 -5 9 21.33 18.30 -2 5 -9 78.99 13.81 2 -5 9 56.84 22.15 2 -5 9 96.94 21.35 -3 5 -9 179.21 26.25 3 -5 9 134.69 27.96 4 4 -9 11.65 14.07 4 4 -9 26.83 17.31 -4 -4 9 17.95 16.19 3 4 -9 316.08 23.08 3 4 -9 297.94 25.45 -3 -4 9 245.70 28.20 2 4 -9 421.35 25.95 2 4 -9 380.40 20.73 -2 -4 9 458.74 30.08 -2 -4 9 385.49 26.67 1 4 -9 220.09 14.44 1 4 -9 251.46 20.96 -1 -4 9 259.39 28.17 -1 -4 9 244.74 23.64 0 4 -9 48.13 8.58 0 -4 9 29.90 16.90 0 -4 9 40.46 13.33 -1 4 -9 45.56 10.06 1 -4 9 57.78 18.56 1 -4 9 26.93 11.90 -2 4 -9 173.06 22.86 2 -4 9 177.78 37.29 2 -4 9 137.47 23.21 -3 4 -9 306.52 30.38 3 -4 9 326.63 30.25 3 -4 9 313.23 50.04 5 3 -9 -12.43 17.25 5 3 -9 -1.99 16.09 4 3 -9 24.55 12.68 4 3 -9 45.20 14.29 -4 -3 9 47.43 16.73 3 3 -9 155.28 17.24 -3 -3 9 112.07 20.98 -3 -3 9 129.86 18.39 2 3 -9 297.23 21.69 2 3 -9 335.20 15.73 -2 -3 9 326.00 24.91 -2 -3 9 301.17 19.59 -2 -3 9 331.79 28.78 1 3 -9 27.53 10.32 -1 -3 9 31.86 11.19 -1 -3 9 3.79 15.01 0 -3 9 62.46 19.02 0 -3 9 67.26 12.65 -1 3 -9 244.89 20.30 1 -3 9 246.46 38.84 1 -3 9 263.70 23.81 -2 3 -9 184.16 21.84 2 -3 9 235.63 39.56 2 -3 9 223.36 24.62 -3 3 -9 143.82 24.66 3 -3 9 122.43 27.38 3 -3 9 93.45 18.31 5 2 -9 102.75 16.91 5 2 -9 55.34 16.07 -5 -2 9 81.44 17.88 4 2 -9 569.73 26.91 4 2 -9 555.47 28.92 -4 -2 9 523.58 32.06 3 2 -9 110.77 14.24 3 2 -9 150.57 15.46 3 2 -9 134.83 13.65 3 2 -9 144.30 16.67 -3 -2 9 160.69 20.59 2 2 -9 18.77 8.84 2 2 -9 23.92 5.60 2 2 -9 20.13 9.23 2 2 -9 28.73 5.84 -2 -2 9 8.00 9.33 -2 -2 9 32.94 10.16 1 2 -9 107.30 15.71 1 2 -9 98.74 14.90 -1 -2 9 93.01 17.98 0 2 -9 551.18 28.65 0 2 -9 547.90 26.99 0 -2 9 574.30 30.58 -1 2 -9 416.49 24.85 -1 2 -9 453.23 28.68 1 -2 9 402.52 29.03 -2 2 -9 106.80 19.99 2 -2 9 64.24 15.44 3 -2 9 16.15 16.43 3 -2 9 12.87 27.80 6 1 -9 8.67 14.52 6 1 -9 7.01 18.12 -6 -1 9 -15.62 16.84 5 1 -9 307.66 26.41 5 1 -9 327.06 24.69 -5 -1 9 350.52 29.50 4 1 -9 193.06 18.17 4 1 -9 203.64 17.29 4 1 -9 166.25 16.95 4 1 -9 173.51 19.03 -4 -1 9 193.24 22.70 3 1 -9 39.17 9.36 3 1 -9 45.53 9.98 3 1 -9 33.35 7.44 3 1 -9 37.06 7.13 -3 -1 9 39.73 10.47 -3 -1 9 33.48 10.66 2 1 -9 38.40 9.96 2 1 -9 41.39 10.05 -2 -1 9 28.92 10.89 1 1 -9 215.55 17.22 1 1 -9 230.11 19.37 -1 -1 9 167.03 19.55 0 1 -9 680.99 29.73 0 1 -9 672.06 31.97 0 -1 9 688.60 34.27 -1 1 -9 335.62 21.65 -1 1 -9 304.87 23.87 1 -1 9 294.03 25.71 -2 1 -9 143.53 21.08 -2 1 -9 152.63 23.17 -3 1 -9 64.42 15.12 3 -1 9 49.66 19.06 6 0 -9 87.05 19.53 6 0 -9 64.34 15.94 -6 0 9 79.47 17.33 5 0 -9 397.84 23.72 5 0 -9 404.31 26.11 -5 0 9 422.39 30.61 4 0 -9 106.31 16.64 4 0 -9 94.67 16.72 4 0 -9 124.61 15.07 4 0 -9 128.29 17.15 -4 0 9 120.53 19.99 3 0 -9 140.48 11.28 3 0 -9 133.13 15.91 3 0 -9 123.38 12.24 -3 0 9 148.80 20.08 2 0 -9 368.73 21.91 -2 0 9 376.62 26.64 1 0 -9 240.48 20.26 1 0 -9 226.97 17.79 -1 0 9 259.82 23.25 0 0 -9 59.92 10.37 0 0 -9 58.54 12.32 0 0 9 44.37 11.81 -1 0 -9 47.76 10.28 -1 0 -9 50.01 14.15 1 0 9 33.34 14.65 -2 0 -9 88.74 16.91 -2 0 -9 134.62 20.83 2 0 9 98.18 20.49 6 -1 -9 39.41 13.64 -6 1 9 55.24 14.82 5 -1 -9 3.09 12.29 5 -1 -9 31.83 14.14 5 -1 -9 -0.18 11.77 4 -1 -9 57.36 19.04 4 -1 -9 50.53 9.23 -4 1 9 77.49 14.58 3 -1 -9 254.71 19.02 3 -1 -9 239.06 20.15 3 -1 -9 245.70 12.46 -3 1 9 257.05 23.12 2 -1 -9 599.43 26.67 2 -1 -9 603.38 30.18 -2 1 9 583.07 33.06 1 -1 -9 382.79 26.02 1 -1 -9 370.25 21.29 -1 1 9 384.64 27.95 0 -1 -9 92.26 15.48 0 1 9 108.58 21.33 -1 -1 -9 153.92 22.82 -1 -1 -9 152.17 19.75 1 1 9 193.56 26.91 -2 -1 -9 83.02 15.21 -2 -1 -9 99.65 18.55 2 1 9 49.41 19.26 6 -2 -9 202.08 25.16 6 -2 -9 207.42 24.47 -6 2 9 199.03 27.30 -6 2 9 205.24 23.85 5 -2 -9 45.31 13.57 5 -2 -9 37.96 12.43 -5 2 9 52.82 11.14 -5 2 9 48.13 14.53 4 -2 -9 140.55 16.58 4 -2 -9 142.79 19.11 -4 2 9 161.08 14.86 -4 2 9 112.40 21.23 3 -2 -9 298.28 22.68 3 -2 -9 285.63 20.01 -3 2 9 257.65 15.13 -3 2 9 332.61 26.82 2 -2 -9 144.38 18.69 2 -2 -9 122.44 15.09 -2 2 9 116.37 20.74 1 -2 -9 98.24 20.43 0 -2 -9 79.27 16.48 0 2 9 67.41 16.55 -1 -2 -9 -3.55 12.14 -1 -2 -9 27.82 15.81 1 2 9 -11.79 17.53 6 -3 -9 87.16 15.37 6 -3 -9 107.34 18.09 -6 3 9 99.00 16.45 -6 3 9 75.19 17.13 5 -3 -9 286.60 25.70 5 -3 -9 218.73 22.52 -5 3 9 250.40 27.15 -5 3 9 222.32 24.89 4 -3 -9 93.98 19.90 4 -3 -9 128.60 17.29 -4 3 9 136.66 15.93 -4 3 9 95.22 16.86 3 -3 -9 104.10 20.72 3 -3 -9 92.20 16.01 -3 3 9 116.49 13.72 -3 3 9 63.65 16.00 2 -3 -9 290.54 26.21 2 -3 -9 291.44 28.75 -2 3 9 266.61 29.11 1 -3 -9 238.12 27.05 1 -3 -9 247.83 19.22 -1 3 9 297.71 30.19 0 -3 -9 145.47 28.29 6 -4 -9 155.76 28.84 6 -4 -9 144.64 24.22 -6 4 9 173.78 26.68 -6 4 9 140.93 26.53 5 -4 -9 173.75 24.84 5 -4 -9 148.95 22.06 -5 4 9 164.44 25.51 -5 4 9 136.49 23.16 4 -4 -9 115.98 14.37 4 -4 -9 181.26 23.99 -4 4 9 128.67 20.02 -4 4 9 151.80 20.87 3 -4 -9 13.64 10.07 3 -4 -9 2.50 13.47 -3 4 9 -7.69 15.21 2 -4 -9 21.76 14.01 2 -4 -9 24.67 10.96 1 -4 -9 24.75 15.98 4 -5 -9 182.28 37.88 4 -5 -9 198.59 22.42 -4 5 9 152.89 29.57 -3 5 9 318.00 34.35 2 5 -10 29.78 14.77 -2 -5 10 18.66 17.68 1 5 -10 21.29 13.65 -1 -5 10 10.90 15.32 -1 -5 10 28.25 19.85 0 -5 10 52.18 15.22 0 -5 10 35.04 23.11 -1 5 -10 127.18 23.94 1 -5 10 168.79 28.67 1 -5 10 116.19 25.69 -3 -4 10 44.25 17.68 2 4 -10 140.44 21.90 -2 -4 10 126.39 24.85 -2 -4 10 115.99 20.59 1 4 -10 95.26 15.58 -1 -4 10 155.62 31.93 0 4 -10 297.13 26.46 0 -4 10 267.59 28.66 -1 4 -10 20.09 12.41 1 -4 10 9.90 14.29 1 -4 10 16.43 23.45 -2 4 -10 32.20 14.83 2 -4 10 47.02 17.52 4 3 -10 -21.06 13.42 -4 -3 10 -10.37 16.37 3 3 -10 17.23 10.33 3 3 -10 1.12 12.29 -3 -3 10 46.33 14.30 2 3 -10 299.18 22.81 -2 -3 10 353.86 27.85 -2 -3 10 288.99 34.99 1 3 -10 144.25 19.29 -1 -3 10 152.21 23.85 0 3 -10 326.30 25.41 0 -3 10 356.53 28.41 0 -3 10 324.43 42.41 -1 3 -10 353.44 25.88 1 -3 10 292.83 27.91 1 -3 10 255.53 44.15 -2 3 -10 50.24 14.23 2 -3 10 18.55 27.94 2 -3 10 30.07 17.82 5 2 -10 78.24 16.95 5 2 -10 103.61 17.32 4 2 -10 148.32 20.89 4 2 -10 172.61 22.78 -4 -2 10 175.44 25.26 3 2 -10 69.45 12.96 3 2 -10 50.57 11.84 3 2 -10 87.93 13.97 -3 -2 10 80.47 15.55 2 2 -10 58.38 12.24 2 2 -10 37.36 12.57 -2 -2 10 44.67 12.71 1 2 -10 195.09 21.30 1 2 -10 160.02 19.37 -1 -2 10 117.56 17.43 0 2 -10 113.74 20.10 0 2 -10 84.07 15.94 0 -2 10 84.72 16.40 -1 2 -10 272.44 28.09 -1 2 -10 294.71 24.57 1 -2 10 358.78 30.88 -2 2 -10 62.34 15.08 2 -2 10 58.94 18.19 5 1 -10 221.13 25.33 5 1 -10 162.43 23.77 -5 -1 10 159.26 21.40 4 1 -10 111.27 20.93 4 1 -10 135.94 18.41 4 1 -10 156.28 21.39 -4 -1 10 136.35 20.12 3 1 -10 305.55 22.83 3 1 -10 277.05 16.29 3 1 -10 260.91 38.92 -3 -1 10 320.73 26.71 2 1 -10 35.02 11.37 2 1 -10 27.63 10.44 -2 -1 10 35.59 11.50 1 1 -10 405.64 26.85 1 1 -10 411.94 25.26 -1 -1 10 366.60 28.81 0 1 -10 503.19 31.09 0 1 -10 443.75 27.57 0 -1 10 481.35 32.07 -1 1 -10 86.33 14.18 -1 1 -10 103.20 22.21 1 -1 10 87.27 19.85 -2 1 -10 61.82 16.25 -2 1 -10 85.29 18.07 2 -1 10 54.68 17.90 5 0 -10 174.45 22.35 5 0 -10 147.81 22.36 -5 0 10 190.33 28.34 4 0 -10 41.43 12.33 4 0 -10 44.27 11.11 4 0 -10 49.76 13.88 -4 0 10 51.86 14.91 3 0 -10 219.45 22.24 3 0 -10 278.36 21.92 -3 0 10 234.14 25.10 2 0 -10 167.66 18.83 2 0 -10 183.56 21.11 -2 0 10 205.08 24.80 1 0 -10 19.13 9.84 1 0 -10 34.56 11.57 -1 0 10 22.97 13.31 0 0 -10 126.74 21.20 0 0 -10 109.98 18.70 -1 0 -10 0.67 14.16 -1 0 -10 -8.22 13.30 1 0 10 55.87 16.97 6 -1 -10 66.75 19.80 -6 1 10 72.57 18.10 5 -1 -10 59.99 15.77 5 -1 -10 54.82 13.90 5 -1 -10 45.89 13.78 -5 1 10 62.34 17.24 4 -1 -10 272.89 20.33 4 -1 -10 253.30 23.41 4 -1 -10 254.76 22.07 -4 1 10 285.77 28.62 3 -1 -10 115.96 17.64 3 -1 -10 125.48 21.46 -3 1 10 157.73 23.70 2 -1 -10 850.74 34.09 2 -1 -10 793.78 38.20 -2 1 10 808.28 41.29 1 -1 -10 204.90 19.02 1 -1 -10 157.31 23.69 -1 1 10 133.49 25.15 0 -1 -10 -5.44 11.72 0 -1 -10 11.32 12.73 0 1 10 33.40 15.63 -1 -1 -10 48.24 15.23 -1 -1 -10 19.26 19.69 6 -2 -10 178.64 29.85 6 -2 -10 124.80 22.11 -6 2 10 130.21 20.74 5 -2 -10 11.33 12.16 5 -2 -10 2.06 13.69 -5 2 10 42.05 13.38 -5 2 10 -6.03 15.08 4 -2 -10 146.85 20.68 4 -2 -10 116.06 22.30 3 -2 -10 28.17 13.18 3 -2 -10 40.42 10.38 -3 2 10 32.87 14.47 2 -2 -10 62.15 15.01 1 -2 -10 133.79 25.33 1 -2 -10 145.49 19.68 -1 2 10 143.63 28.20 0 -2 -10 56.10 13.13 0 -2 -10 42.73 17.74 5 -3 -10 352.50 26.37 5 -3 -10 297.23 31.11 -5 3 10 296.37 32.87 4 -3 -10 -3.43 11.84 4 -3 -10 21.86 14.39 -4 3 10 2.62 15.59 3 -3 -10 183.55 26.24 3 -3 -10 153.46 19.47 -3 3 10 113.27 19.01 2 -3 -10 7.56 11.70 2 -3 -10 16.68 14.06 -2 3 10 -0.66 16.81 -1 3 10 7.71 27.59 4 -4 -10 -5.10 13.73 4 -4 -10 -7.91 15.72 -4 4 10 -3.92 17.54 3 -4 -10 81.34 14.85 -3 4 10 78.51 20.11 2 4 -11 182.39 32.16 -2 -4 11 261.64 30.65 1 4 -11 156.31 26.24 -1 -4 11 195.43 31.66 -1 -4 11 140.36 26.78 0 4 -11 36.63 14.61 0 -4 11 -8.99 26.13 0 -4 11 35.08 18.27 3 3 -11 85.51 15.51 2 3 -11 130.58 20.09 -2 -3 11 149.45 27.29 -2 -3 11 153.05 21.57 1 3 -11 241.06 25.74 -1 -3 11 278.73 31.81 -1 -3 11 198.70 31.03 0 3 -11 445.05 31.60 0 -3 11 384.82 51.35 0 -3 11 456.07 35.18 1 -3 11 79.09 28.80 4 2 -11 70.04 17.31 -4 -2 11 100.71 32.55 3 2 -11 133.71 22.94 3 2 -11 144.65 23.32 -3 -2 11 101.25 20.02 2 2 -11 22.89 13.29 2 2 -11 33.44 13.83 -2 -2 11 33.21 14.86 1 2 -11 47.36 14.78 1 2 -11 33.76 14.47 0 2 -11 90.37 17.84 0 -2 11 106.96 18.86 -1 2 -11 208.87 27.06 1 -2 11 233.29 32.28 4 1 -11 280.32 26.85 -4 -1 11 304.63 33.81 3 1 -11 153.85 24.19 -3 -1 11 129.14 26.16 2 1 -11 48.97 14.75 -2 -1 11 32.71 15.61 1 1 -11 198.29 22.77 1 1 -11 166.74 26.66 -1 -1 11 215.74 27.89 0 1 -11 -0.47 14.59 0 1 -11 30.70 13.37 0 -1 11 12.05 16.55 4 0 -11 68.90 15.96 4 0 -11 72.10 14.83 -4 0 11 87.54 17.72 3 0 -11 11.58 11.86 -3 0 11 -2.51 15.48 2 0 -11 213.10 23.13 2 0 -11 165.57 25.46 -2 0 11 190.16 28.05 1 0 -11 160.01 22.10 1 0 -11 153.06 27.20 -1 0 11 141.97 27.94 0 0 -11 38.42 15.19 0 0 -11 49.93 15.45 0 0 11 86.05 21.07 5 -1 -11 14.05 17.60 5 -1 -11 10.78 20.42 -5 1 11 4.89 17.98 4 -1 -11 -4.72 14.30 4 -1 -11 -14.90 13.00 -4 1 11 -27.86 15.84 3 -1 -11 154.42 25.81 3 -1 -11 204.83 22.56 -3 1 11 207.97 28.65 2 -1 -11 399.14 26.11 2 -1 -11 349.67 30.58 -2 1 11 338.40 34.81 1 -1 -11 9.60 14.12 1 -1 -11 29.94 15.76 -1 1 11 9.03 17.92 4 -2 -11 11.77 15.92 4 -2 -11 6.68 13.57 -4 2 11 27.69 17.92 3 -2 -11 182.22 28.40 3 -2 -11 216.46 24.83 -3 2 11 219.91 31.99 2 -2 -11 127.60 23.28 2 -2 -11 177.13 28.43 -2 2 11 129.14 23.74 2 1 -12 84.11 19.84 2 1 -12 49.50 18.91 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6890 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71140 6.291 6.854 9.268 96.324 105.054 113.412 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 70763 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Ni1 Ni 1.0000 0.5000 1.0000 0.00925(15) Uani 1 2 d S T P O2 O 0.0777(3) 0.0839(3) 0.2630(2) 0.0149(4) Uani 1 1 d . . . O3 O 1.2214(3) 0.7637(3) 0.9276(2) 0.0134(4) Uani 1 1 d . . . H3A H 1.1315 0.8080 0.8631 0.020 Uiso 1 1 d GR . . H3B H 1.2967 0.7220 0.8723 0.020 Uiso 1 1 d GR . . O4 O 0.8204(3) 0.6848(3) 1.0418(2) 0.0125(4) Uani 1 1 d . . . H4 H 0.9206 0.8038 1.1009 0.019 Uiso 1 1 calc GR . . O1 O 0.4223(4) 0.2301(3) 0.2022(2) 0.0163(4) Uani 1 1 d . . . H1 H 0.3238 0.1938 0.1147 0.024 Uiso 1 1 calc R . . N1 N 0.7619(4) 0.3608(4) 0.7726(2) 0.0108(4) Uani 1 1 d . . . C3 C 0.7166(5) 0.2954(4) 0.5038(3) 0.0120(5) Uani 1 1 d . . . H3 H 0.7894 0.2962 0.4280 0.014 Uiso 1 1 calc R . . C1 C 0.3074(5) 0.1746(4) 0.2952(3) 0.0122(5) Uani 1 1 d . . . C4 C 0.8565(5) 0.3585(4) 0.6575(3) 0.0120(5) Uani 1 1 d . . . H4A H 1.0248 0.4018 0.6833 0.014 Uiso 1 1 calc R . . C6 C 0.3638(5) 0.2222(4) 0.5810(3) 0.0117(5) Uani 1 1 d . . . H6 H 0.1949 0.1724 0.5579 0.014 Uiso 1 1 calc R . . C5 C 0.5168(5) 0.2890(4) 0.7324(3) 0.0130(5) Uani 1 1 d . . . H5 H 0.4474 0.2842 0.8102 0.016 Uiso 1 1 calc R . . C2 C 0.4649(5) 0.2303(4) 0.4632(3) 0.0099(5) Uani 1 1 d . . . 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 Ni1 0.0084(3) 0.0120(3) 0.0073(2) 0.00171(18) 0.00197(18) 0.0050(2) O2 0.0119(10) 0.0164(10) 0.0134(10) 0.0025(8) 0.0017(8) 0.0053(8) O3 0.0118(9) 0.0172(10) 0.0135(9) 0.0055(8) 0.0053(8) 0.0076(8) O4 0.0111(9) 0.0130(9) 0.0108(9) -0.0008(7) 0.0019(7) 0.0051(8) O1 0.0159(10) 0.0254(11) 0.0097(9) 0.0052(8) 0.0033(8) 0.0116(9) N1 0.0134(11) 0.0103(11) 0.0097(10) 0.0021(8) 0.0036(9) 0.0063(9) C3 0.0134(13) 0.0123(13) 0.0119(13) 0.0036(10) 0.0062(10) 0.0058(11) C1 0.0152(13) 0.0102(12) 0.0137(13) 0.0028(10) 0.0043(11) 0.0086(11) C4 0.0110(13) 0.0129(13) 0.0128(13) 0.0027(10) 0.0048(10) 0.0055(11) C6 0.0105(12) 0.0115(12) 0.0132(13) 0.0011(10) 0.0025(10) 0.0063(11) C5 0.0116(13) 0.0153(13) 0.0144(13) 0.0025(10) 0.0062(11) 0.0074(11) C2 0.0114(12) 0.0069(11) 0.0130(13) 0.0035(10) 0.0035(10) 0.0056(10) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' 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 O3 Ni1 O3 180.00(11) 2_767 . O4 Ni1 O3 86.81(7) 2_767 2_767 O4 Ni1 O3 93.19(7) 2_767 . O4 Ni1 O3 93.19(7) . 2_767 O4 Ni1 O3 86.81(7) . . O4 Ni1 O4 180.00(7) . 2_767 O4 Ni1 N1 88.14(8) . 2_767 O4 Ni1 N1 88.14(8) 2_767 . O4 Ni1 N1 91.86(8) 2_767 2_767 O4 Ni1 N1 91.86(8) . . N1 Ni1 O3 90.75(8) 2_767 . N1 Ni1 O3 89.25(8) . . N1 Ni1 O3 89.25(8) 2_767 2_767 N1 Ni1 O3 90.75(8) . 2_767 N1 Ni1 N1 180.00(13) 2_767 . Ni1 O3 H3A 110.9 . . Ni1 O3 H3B 110.8 . . H3A O3 H3B 103.1 . . Ni1 O4 H4 109.5 . . C1 O1 H1 109.5 . . C4 N1 Ni1 119.26(18) . . C5 N1 Ni1 123.21(17) . . C5 N1 C4 117.3(2) . . C4 C3 H3 120.4 . . C4 C3 C2 119.1(2) . . C2 C3 H3 120.4 . . O2 C1 O1 126.4(2) . . O2 C1 C2 117.6(2) . . O1 C1 C2 115.9(2) . . N1 C4 C3 123.2(2) . . N1 C4 H4A 118.4 . . C3 C4 H4A 118.4 . . C5 C6 H6 120.4 . . C5 C6 C2 119.2(2) . . C2 C6 H6 120.4 . . N1 C5 C6 123.0(2) . . N1 C5 H5 118.5 . . C6 C5 H5 118.5 . . C3 C2 C1 120.6(2) . . C3 C2 C6 118.0(2) . . C6 C2 C1 121.4(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O3 2.0947(18) . Ni1 O3 2.0947(18) 2_767 Ni1 O4 2.0653(18) 2_767 Ni1 O4 2.0653(18) . Ni1 N1 2.087(2) 2_767 Ni1 N1 2.087(2) . O2 C1 1.256(3) . O3 H3A 0.8749 . O3 H3B 0.8750 . O4 H4 0.8200 . O1 H1 0.8200 . O1 C1 1.256(3) . N1 C4 1.348(3) . N1 C5 1.344(3) . C3 H3 0.9300 . C3 C4 1.375(4) . C3 C2 1.389(4) . C1 C2 1.519(4) . C4 H4A 0.9300 . C6 H6 0.9300 . C6 C5 1.379(4) . C6 C2 1.391(4) . C5 H5 0.9300 .