#------------------------------------------------------------------------------ #$Date: 2021-10-03 22:54:18 +0300 (Sun, 03 Oct 2021) $ #$Revision: 269490 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519068.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_4519068 loop_ _publ_author_name 'Ankade, Shidheshwar B.' 'Samal, Pragnya Paramita' 'Soni, Vineeta' 'Gonnade, Rajesh G.' 'Krishnamurty, Sailaja' 'Punji, Benudhar' _publ_section_title ; Ni(II)-Catalyzed Intramolecular C--H/C--H Oxidative Coupling: An Efficient Route to Functionalized Cycloindolones and Indenoindolones ; _journal_issue 19 _journal_name_full 'ACS Catalysis' _journal_page_first 12384 _journal_page_last 12393 _journal_paper_doi 10.1021/acscatal.1c03314 _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'C14 H18 N2 Ni O6' _chemical_formula_sum 'C14 H18 N2 Ni O6' _chemical_formula_weight 369.01 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 92.8820(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.2287(7) _cell_length_b 12.7164(5) _cell_length_c 8.0895(3) _cell_measurement_reflns_used 9803 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.95 _cell_measurement_theta_min 4.53 _cell_volume 1564.58(11) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'SAINT (Bruker, 2016)' _computing_molecular_graphics 'Bruker SHELXTL, Mercury 2020.20' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Photon II CPAD Area Detector' _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 20123 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.945 _diffrn_reflns_theta_min 4.532 _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'Incoatech I\mS HB' _exptl_absorpt_coefficient_mu 2.097 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.567 _exptl_crystal_description block _exptl_crystal_F_000 768 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.170 _refine_diff_density_max 0.431 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 114 _refine_ls_number_reflns 1597 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0317 _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^)+(0.0370P)^2^+2.6868P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.0843 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1551 _reflns_number_total 1597 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c03314_si_003.cif _cod_data_source_block Comp_1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4519068 _shelx_shelxl_version_number 2018/3 _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_min 0.545 _shelx_estimated_absorpt_t_max 0.717 _shelx_res_file ; TITL cu_SA_NIOACBPY_0m_a.res in C2/c cu_SA_NIOACBPY_0m_a.res created by SHELXL-2018/3 at 13:04:38 on 26-Jun-2021 CELL 1.54178 15.2287 12.7164 8.0895 90.000 92.882 90.000 ZERR 4.000 0.0007 0.0005 0.0003 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N Ni O UNIT 56 72 8 4 24 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 30 OMIT 0 0 4 OMIT -3 1 2 OMIT -3.0 150 ACTA BOND $H FMAP 2 CONF SIZE 0.33 0.22 0.17 PLAN 5 TEMP -173.370 WGHT 0.037000 2.686800 FVAR 0.70315 NI1 4 0.500000 0.772046 0.250000 10.50000 0.02077 0.01479 = 0.01382 0.00000 0.00338 0.00000 O1 5 0.444114 0.770874 0.479249 11.00000 0.02867 0.01778 = 0.01724 0.00096 0.00717 0.00251 O2 5 0.398063 0.937294 0.484675 11.00000 0.04249 0.01965 = 0.01923 -0.00059 0.00514 0.00657 O3 5 0.593453 0.883056 0.325966 11.00000 0.02705 0.01785 = 0.01633 -0.00145 0.00295 -0.00170 H3A 2 0.583825 0.928874 0.383741 11.00000 0.03447 H3B 2 0.600958 0.907916 0.234304 11.00000 0.04978 N1 3 0.422541 0.646311 0.170676 11.00000 0.02144 0.01791 = 0.01640 -0.00033 0.00571 -0.00102 C1 1 0.345545 0.653181 0.083416 11.00000 0.02371 0.02304 = 0.01981 -0.00160 0.00505 -0.00109 AFIX 43 H1 2 0.320774 0.720816 0.063236 11.00000 -1.20000 AFIX 0 C2 1 0.300595 0.565909 0.021464 11.00000 0.02546 0.03118 = 0.02337 -0.00333 0.00391 -0.00447 AFIX 43 H2 2 0.245722 0.573189 -0.038650 11.00000 -1.20000 AFIX 0 C3 1 0.337745 0.467764 0.049453 11.00000 0.03113 0.02488 = 0.02691 -0.00739 0.00764 -0.00870 AFIX 43 H3 2 0.308844 0.406438 0.007408 11.00000 -1.20000 AFIX 0 C4 1 0.417294 0.459583 0.139123 11.00000 0.03147 0.01851 = 0.02610 -0.00309 0.00928 -0.00250 AFIX 43 H4 2 0.443912 0.392853 0.158478 11.00000 -1.20000 AFIX 0 C5 1 0.457602 0.550719 0.200416 11.00000 0.02449 0.01748 = 0.01728 -0.00074 0.00853 -0.00109 C6 1 0.409278 0.848151 0.548705 11.00000 0.02308 0.02140 = 0.01719 -0.00120 0.00370 0.00029 C7 1 0.376847 0.830220 0.720525 11.00000 0.04123 0.02833 = 0.02097 0.00043 0.01277 0.00471 AFIX 137 H7A 2 0.322156 0.789516 0.712443 11.00000 -1.50000 H7B 2 0.365994 0.898178 0.772859 11.00000 -1.50000 H7C 2 0.421422 0.791370 0.787378 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_SA_NIOACBPY_0m_a.res in C2/c REM wR2 = 0.084266, GooF = S = 1.08939, Restrained GooF = 1.08939 for all data REM R1 = 0.031677 for 1551 Fo > 4sig(Fo) and 0.032305 for all 1597 data REM 114 parameters refined using 0 restraints END WGHT 0.0370 2.6868 REM Highest difference peak 0.431, deepest hole -0.452, 1-sigma level 0.058 Q1 1 0.4311 0.7741 0.2407 11.00000 0.05 0.43 Q2 1 0.4589 0.6819 0.1948 11.00000 0.05 0.28 Q3 1 0.5000 0.5464 0.2500 10.50000 0.05 0.25 Q4 1 0.4424 0.5065 0.1453 11.00000 0.05 0.25 Q5 1 0.3928 0.8373 0.6357 11.00000 0.05 0.23 ; _shelx_res_checksum 6793 _shelx_hkl_file ; -6 0 0 1599.94 96.79 -6 0 0 1630.44 96.29 -6 0 0 1531.45 96.69 -6 0 0 1511.65 97.29 6 0 0 1578.64 97.39 6 0 0 1649.73 96.59 6 0 0 1549.74 96.79 6 0 0 1510.45 96.79 6 0 0 1575.84 97.19 6 0 0 1659.93 97.19 -6 0 0 1620.04 97.89 8 0 0 107.69 8.20 8 0 0 118.69 8.70 8 0 0 127.19 8.70 8 0 0 113.99 8.80 -8 0 0 125.09 9.00 -8 0 0 105.99 8.00 -8 0 0 115.89 8.40 -8 0 0 117.39 8.20 -8 0 0 117.09 7.50 8 0 0 119.29 8.50 -10 0 0 2951.90 160.88 -10 0 0 2534.45 158.08 10 0 0 2749.82 159.78 10 0 0 2474.15 159.18 -10 0 0 2561.74 159.28 -10 0 0 2633.64 159.08 10 0 0 2437.36 159.48 10 0 0 2612.14 159.18 -10 0 0 2436.66 158.98 12 0 0 2567.54 161.48 -12 0 0 2505.75 160.58 -12 0 0 2779.42 160.98 12 0 0 2420.36 161.68 -12 0 0 2645.34 161.18 -12 0 0 2454.65 161.88 -12 0 0 2579.54 160.78 12 0 0 2704.43 160.98 12 0 0 2633.54 161.58 -12 0 0 2729.23 162.28 12 0 0 2805.82 161.78 14 0 0 404.26 28.00 14 0 0 388.16 28.20 -14 0 0 441.66 27.60 -14 0 0 423.76 26.90 -14 0 0 415.06 28.70 14 0 0 411.16 28.10 -14 0 0 409.26 28.60 16 0 0 0.20 1.10 -16 0 0 -0.70 2.10 16 0 0 -1.50 1.00 -16 0 0 1.30 1.70 16 0 0 -0.90 1.00 -16 0 0 0.20 1.50 -16 0 0 -0.30 3.00 18 0 0 72.49 5.90 18 0 0 71.59 6.30 -18 0 0 76.59 6.70 -1 -1 0 21.00 1.60 -1 -1 0 22.50 1.50 1 -1 0 20.60 1.60 -1 -1 0 27.90 2.00 1 1 0 25.90 1.80 -1 1 0 26.90 1.80 -1 1 0 23.00 1.70 -1 1 0 20.60 1.60 -1 1 0 25.80 1.60 1 1 0 25.30 2.00 3 -1 0 466.35 26.00 3 -1 0 447.26 25.80 -3 -1 0 447.36 25.70 -3 -1 0 439.36 25.60 3 -1 0 387.36 26.00 -3 -1 0 423.96 26.20 3 -1 0 362.46 25.70 -3 -1 0 409.16 25.80 3 1 0 444.26 25.80 -3 1 0 389.16 25.80 -3 1 0 416.86 25.80 3 1 0 389.26 25.70 -3 1 0 425.56 25.70 -3 1 0 406.56 25.90 -3 1 0 416.76 25.60 3 1 0 417.36 26.40 5 -1 0 5784.12 369.06 5 -1 0 6762.72 368.56 -5 -1 0 5626.34 368.16 5 -1 0 6316.87 368.76 5 1 0 6380.96 368.26 5 1 0 5850.31 368.66 5 1 0 5740.63 368.66 7 -1 0 127.89 8.60 7 -1 0 120.39 8.70 7 -1 0 128.19 8.40 7 -1 0 109.59 8.30 -7 -1 0 126.59 7.70 -7 -1 0 130.59 8.50 -7 -1 0 126.09 9.10 7 -1 0 119.99 8.70 7 -1 0 120.89 8.30 7 1 0 135.79 8.90 7 1 0 105.99 8.40 -7 1 0 125.79 8.90 7 1 0 114.69 9.20 7 1 0 126.19 8.50 -7 1 0 122.39 8.30 7 1 0 125.79 7.90 7 1 0 102.39 8.70 -7 1 0 120.29 8.30 -9 -1 0 3774.72 226.18 -9 -1 0 3775.22 224.18 9 -1 0 3811.22 225.68 9 -1 0 4113.99 225.78 -9 -1 0 3520.45 225.08 9 -1 0 3836.92 225.18 -9 -1 0 3685.93 225.18 9 -1 0 3859.41 225.18 -9 -1 0 3649.73 225.28 9 -1 0 3598.54 225.28 9 -1 0 3539.05 224.98 -9 1 0 3638.44 225.78 -9 1 0 3589.04 225.38 -9 1 0 3645.14 224.98 9 1 0 3669.13 225.28 9 1 0 3725.33 225.78 -9 1 0 3480.55 225.08 9 1 0 3689.23 225.28 9 1 0 3574.64 226.28 9 1 0 3728.03 225.78 -9 1 0 3619.94 224.38 -11 -1 0 366.36 25.30 -11 -1 0 405.76 25.60 -11 -1 0 376.46 25.50 11 -1 0 400.26 26.20 11 -1 0 433.56 25.80 11 -1 0 411.06 26.10 -11 -1 0 378.76 26.70 -11 -1 0 351.76 26.40 11 -1 0 422.06 25.80 11 -1 0 386.76 26.30 11 -1 0 367.06 25.10 -11 -1 0 406.26 25.80 11 -1 0 380.06 25.90 -11 1 0 390.56 25.70 -11 1 0 405.76 25.40 -11 1 0 359.86 25.40 11 1 0 405.36 26.30 11 1 0 376.86 26.10 -11 1 0 373.66 25.00 11 1 0 439.96 29.50 -11 1 0 358.36 26.60 -11 1 0 423.06 33.40 -11 1 0 392.26 26.40 13 -1 0 41.40 5.10 -13 -1 0 50.49 6.10 -13 -1 0 49.60 4.90 -13 -1 0 53.99 5.20 13 -1 0 34.60 4.80 -13 -1 0 58.89 6.40 -13 -1 0 55.39 5.20 13 -1 0 47.40 5.90 13 -1 0 53.39 5.60 -13 -1 0 39.80 6.00 -13 -1 0 44.30 4.50 -13 1 0 47.90 5.50 13 1 0 36.60 6.40 13 1 0 32.40 5.00 -13 1 0 43.80 4.40 -13 1 0 33.00 5.70 -13 1 0 42.20 4.70 13 1 0 40.80 5.90 13 1 0 44.30 5.40 -15 -1 0 56.79 7.00 -15 -1 0 57.39 5.80 -15 -1 0 60.59 6.80 15 -1 0 54.39 6.40 15 -1 0 58.89 6.20 15 -1 0 62.29 7.00 15 1 0 59.09 6.40 -15 1 0 57.69 7.30 15 1 0 48.90 7.40 15 1 0 53.39 6.70 -15 1 0 57.19 6.70 -15 1 0 52.79 7.10 -17 -1 0 58.29 6.40 17 -1 0 56.49 6.60 17 -1 0 55.59 6.10 -17 -1 0 52.09 5.40 -17 1 0 64.99 6.60 17 1 0 59.29 5.90 -17 1 0 58.79 5.40 17 1 0 57.59 5.40 17 1 0 63.79 6.00 0 -2 0 270.47 18.90 0 -2 0 307.37 19.50 0 2 0 328.77 18.90 0 2 0 288.27 19.00 0 2 0 353.56 19.40 -4 -2 0 3513.15 227.88 4 -2 0 3812.32 227.28 4 -2 0 4216.58 227.88 4 -2 0 3830.42 227.78 4 -2 0 3601.44 227.28 4 -2 0 3607.44 227.58 -4 2 0 3754.92 227.08 4 2 0 3586.14 227.58 -6 -2 0 1989.90 118.49 6 -2 0 1833.22 118.29 -6 -2 0 1826.82 117.59 -6 -2 0 1967.20 119.09 6 -2 0 1986.10 118.69 6 -2 0 2057.29 118.29 6 -2 0 2041.40 118.69 -6 2 0 1885.91 118.39 -6 2 0 1981.10 117.99 6 2 0 1951.70 118.79 -6 2 0 1887.81 118.49 -6 2 0 1875.31 118.59 6 2 0 1982.10 119.69 6 2 0 1848.02 118.39 -6 2 0 1958.60 118.19 8 -2 0 1396.46 84.39 8 -2 0 1203.98 84.19 -8 -2 0 1321.87 84.39 -8 -2 0 1475.75 85.59 -8 -2 0 1505.35 84.69 8 -2 0 1392.46 84.49 8 -2 0 1444.86 84.59 8 -2 0 1384.96 84.79 8 2 0 1396.06 85.09 8 2 0 1441.96 84.89 -8 2 0 1341.87 84.89 -8 2 0 1444.86 83.89 -8 2 0 1304.67 84.19 -8 2 0 1195.08 84.39 8 2 0 1353.46 85.99 -10 -2 0 106.49 7.90 10 -2 0 107.39 7.70 10 -2 0 94.09 7.50 10 -2 0 100.39 8.00 10 -2 0 98.19 7.70 -10 -2 0 97.09 8.60 -10 -2 0 97.89 7.60 10 -2 0 110.59 8.30 -10 2 0 90.99 7.30 -10 2 0 91.69 8.10 -10 2 0 103.79 6.90 -10 2 0 103.29 7.90 10 2 0 101.49 8.00 10 2 0 105.79 8.50 -12 -2 0 358.96 24.70 -12 -2 0 376.76 26.20 -12 -2 0 392.46 25.00 12 -2 0 375.66 25.50 12 -2 0 373.26 25.80 12 -2 0 339.47 25.10 -12 -2 0 430.76 25.50 12 -2 0 364.56 24.40 12 -2 0 378.16 25.60 -12 -2 0 390.96 25.20 12 -2 0 362.56 24.40 -12 -2 0 418.36 26.80 12 -2 0 404.06 25.00 -12 2 0 326.27 24.30 12 2 0 388.16 25.70 -12 2 0 381.56 25.80 12 2 0 414.96 26.70 12 2 0 353.96 26.00 12 2 0 395.46 25.70 -12 2 0 402.26 31.00 -12 2 0 347.97 26.70 -12 2 0 391.76 24.80 12 2 0 380.26 26.40 -12 2 0 350.16 26.20 -14 -2 0 1063.39 62.69 -14 -2 0 954.20 63.49 14 -2 0 1111.09 63.19 -14 -2 0 931.21 62.89 14 -2 0 1018.20 62.59 -14 -2 0 995.90 61.69 -14 -2 0 1003.10 62.69 14 -2 0 994.20 62.19 -14 -2 0 996.90 61.49 -14 2 0 989.40 62.79 -14 2 0 862.11 62.89 14 2 0 936.01 62.89 14 2 0 1000.90 62.29 14 2 0 940.21 63.29 14 2 0 950.70 62.99 14 2 0 983.60 62.59 -16 -2 0 818.12 54.59 -16 -2 0 702.43 52.89 -16 -2 0 838.62 53.99 16 -2 0 805.62 53.39 -16 -2 0 858.01 52.29 16 2 0 909.01 54.19 16 2 0 922.71 53.89 -16 2 0 830.42 53.49 -16 2 0 881.81 54.39 18 -2 0 303.77 20.80 18 -2 0 279.87 20.50 -18 -2 0 298.57 20.50 18 2 0 285.97 20.20 -18 2 0 345.77 21.00 18 2 0 341.47 20.60 3 -3 0 150.78 9.60 -3 -3 0 125.09 9.20 -3 -3 0 134.79 9.70 3 -3 0 146.09 9.30 -3 3 0 144.19 9.30 3 3 0 137.29 9.40 -3 3 0 155.68 9.80 3 3 0 147.79 9.70 -3 3 0 147.89 9.10 5 -3 0 5.10 1.20 -5 -3 0 6.20 1.60 -5 -3 0 7.20 1.40 5 -3 0 6.20 1.60 5 -3 0 6.10 1.60 -5 3 0 6.50 0.90 -5 3 0 7.60 1.30 -5 3 0 5.20 0.90 5 3 0 4.30 1.30 5 3 0 5.30 1.40 5 3 0 8.90 2.40 -5 3 0 6.60 1.50 7 -3 0 5.80 1.30 -7 -3 0 5.50 1.50 -7 -3 0 5.20 2.10 -7 -3 0 5.90 1.20 7 -3 0 6.70 1.50 7 -3 0 5.10 1.50 -7 3 0 7.00 1.80 7 3 0 8.80 2.00 -7 3 0 7.10 1.20 7 3 0 7.70 1.20 7 3 0 7.60 1.70 -7 3 0 5.50 1.50 -7 3 0 8.70 1.60 -9 -3 0 485.15 30.30 9 -3 0 453.05 29.00 9 -3 0 419.86 28.60 9 -3 0 461.15 28.80 9 -3 0 448.26 28.60 9 -3 0 444.46 28.60 -9 -3 0 461.65 28.60 -9 -3 0 453.55 28.70 -9 -3 0 467.25 29.00 9 3 0 461.15 29.60 -9 3 0 445.66 29.00 9 3 0 444.26 29.00 -9 3 0 413.36 28.70 -9 3 0 450.15 28.00 -9 3 0 430.16 28.20 -11 -3 0 277.77 20.20 -11 -3 0 282.07 20.50 11 -3 0 276.67 18.90 11 -3 0 305.67 19.70 -11 -3 0 248.08 19.00 11 -3 0 290.47 20.00 11 -3 0 269.37 19.20 11 -3 0 267.07 20.70 11 -3 0 296.27 19.60 -11 -3 0 267.27 18.90 11 -3 0 300.17 19.00 -11 -3 0 292.47 19.30 11 3 0 297.67 21.40 11 3 0 343.27 29.10 -11 3 0 294.17 21.20 11 3 0 251.87 19.20 -11 3 0 277.97 29.90 -11 3 0 285.17 18.20 11 3 0 279.77 19.90 -11 3 0 284.47 20.70 11 3 0 272.17 20.80 -13 -3 0 19.40 3.40 -13 -3 0 12.40 2.50 -13 -3 0 13.40 2.80 13 -3 0 8.80 3.30 13 -3 0 9.10 3.20 -13 -3 0 13.10 3.00 13 -3 0 13.60 3.60 -13 -3 0 15.10 4.40 -13 -3 0 17.50 4.50 -13 -3 0 16.70 4.00 13 -3 0 13.00 3.00 13 3 0 12.90 3.60 13 3 0 6.60 2.70 -13 3 0 11.60 3.60 -13 3 0 12.50 3.70 -13 3 0 12.00 4.20 13 3 0 11.80 4.40 13 3 0 16.80 4.30 13 3 0 16.30 4.90 -15 -3 0 -0.50 1.40 -15 -3 0 0.10 2.30 15 -3 0 3.10 1.40 -15 -3 0 0.80 1.90 -15 -3 0 -0.30 1.30 15 -3 0 0.70 1.30 15 -3 0 1.20 1.30 -15 -3 0 2.30 1.20 -15 -3 0 0.50 1.20 15 3 0 0.70 1.00 15 3 0 3.90 1.40 15 3 0 2.30 1.30 -15 3 0 -1.70 1.50 -15 3 0 0.50 2.50 -15 3 0 -1.20 2.40 -17 -3 0 28.40 4.30 -17 -3 0 25.10 4.20 17 -3 0 31.60 3.70 -17 -3 0 22.00 3.20 -17 -3 0 27.10 4.20 17 -3 0 33.30 4.20 17 3 0 31.60 4.50 -17 3 0 27.90 4.70 17 3 0 32.30 3.80 -17 3 0 29.70 3.80 0 -4 0 4.10 0.60 0 -4 0 2.60 0.80 0 4 0 2.90 0.50 0 4 0 3.90 1.30 0 4 0 4.20 0.70 0 4 0 3.90 1.20 2 -4 0 1982.40 130.29 2 -4 0 2090.49 131.19 -2 -4 0 2008.20 130.09 -2 4 0 2157.88 130.29 2 4 0 2166.08 130.89 2 4 0 2277.37 130.59 2 4 0 2284.87 129.79 4 -4 0 8378.96 509.05 -6 -4 0 4600.04 297.77 -6 -4 0 4456.45 298.97 -6 -4 0 4870.11 298.27 6 -4 0 4976.50 298.57 6 -4 0 4730.93 298.07 6 -4 0 4990.00 298.87 6 -4 0 4958.50 298.27 6 -4 0 5174.78 298.17 -6 4 0 5253.07 298.37 -6 4 0 4841.32 297.57 -6 4 0 4811.82 298.77 6 4 0 4829.52 298.47 -6 4 0 4916.21 297.77 6 4 0 5205.78 298.37 -8 -4 0 194.58 13.40 -8 -4 0 200.28 14.40 8 -4 0 194.28 13.20 8 -4 0 192.08 13.60 -8 -4 0 182.48 13.10 8 -4 0 198.18 13.30 -8 -4 0 180.28 12.90 8 -4 0 216.48 13.30 8 4 0 181.58 13.50 8 4 0 199.98 14.10 -8 4 0 204.28 12.70 -8 4 0 202.68 13.40 -10 -4 0 25.00 3.20 10 -4 0 23.70 3.00 10 -4 0 23.40 3.20 10 -4 0 21.70 3.10 10 -4 0 27.60 3.20 10 -4 0 21.50 4.00 -10 -4 0 18.80 2.70 -10 -4 0 16.70 2.70 -10 -4 0 22.70 4.00 10 4 0 23.70 5.00 -10 4 0 22.80 4.10 -10 4 0 20.90 6.20 -10 4 0 18.40 5.00 10 4 0 15.80 4.20 -10 4 0 21.50 2.40 10 4 0 30.70 4.00 12 -4 0 16.80 2.90 -12 -4 0 16.10 3.00 -12 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22.70 2 2 9 373.06 21.30 2 2 9 305.57 21.60 2 2 9 354.66 27.20 -2 2 -9 300.17 22.50 -2 2 -9 311.87 21.70 2 2 9 294.87 22.70 2 2 9 343.87 23.00 4 -2 9 11.50 2.50 -4 -2 -9 7.40 2.50 4 -2 9 11.20 2.90 4 -2 9 6.30 2.30 4 2 9 9.30 2.00 4 2 9 12.10 3.40 -4 2 -9 8.30 2.40 4 2 9 8.10 4.10 4 2 9 11.60 2.70 -4 2 -9 9.90 2.70 4 2 9 9.00 2.30 6 -2 9 1.30 0.70 6 -2 9 -0.30 0.90 6 -2 9 0.70 0.70 -6 -2 -9 0.50 0.90 -6 -2 -9 0.00 0.80 -6 2 -9 0.90 1.20 -6 2 -9 -0.20 1.10 -6 2 -9 -1.00 1.00 6 2 9 0.80 0.70 6 2 9 -0.40 1.10 6 2 9 1.10 0.80 -7 -3 9 26.70 2.70 7 -3 -9 17.70 3.20 7 -3 -9 24.20 3.00 -7 -3 9 26.80 2.70 7 3 -9 19.30 3.20 7 3 -9 21.50 2.70 -7 3 9 21.80 4.00 -7 3 9 20.80 2.40 -7 3 9 20.90 2.70 -7 3 9 28.10 2.80 5 -3 -9 90.89 7.30 -5 -3 9 90.19 7.40 5 -3 -9 89.79 7.70 -5 -3 9 90.59 7.10 5 -3 -9 96.89 7.50 -5 -3 9 114.19 7.50 5 3 -9 106.29 8.60 -5 3 9 96.09 7.20 -5 3 9 93.79 7.50 -5 3 9 85.59 7.70 5 3 -9 113.79 7.40 5 3 -9 104.39 7.50 5 3 -9 100.39 8.60 -5 3 9 105.19 8.10 -3 -3 9 920.71 66.39 3 -3 -9 1216.08 66.69 3 -3 -9 1038.50 66.79 -3 -3 9 1037.40 67.99 3 -3 -9 1110.89 67.29 3 -3 -9 991.80 66.59 -3 -3 9 1054.69 66.69 -3 -3 9 1045.00 66.39 -3 3 9 1127.89 67.59 -3 3 9 1170.38 66.59 3 3 -9 1050.59 67.89 -3 3 9 1060.29 66.49 3 3 -9 1095.29 66.79 -3 3 9 1076.79 66.29 -3 3 9 958.80 71.19 3 3 -9 1109.49 67.49 3 3 -9 1172.58 66.79 -1 -3 9 770.32 54.89 -1 -3 9 790.62 54.29 1 -3 -9 847.22 54.99 -1 -3 9 768.52 54.59 -1 -3 9 804.02 56.09 -1 3 9 1027.00 56.39 1 3 -9 993.80 55.49 -1 3 9 941.71 61.09 1 3 -9 925.31 56.19 1 3 -9 942.21 55.19 -1 3 9 808.42 54.59 -1 3 9 923.81 56.29 1 -3 9 659.23 48.00 1 -3 9 773.12 47.80 1 -3 9 725.43 48.50 -1 -3 -9 724.03 47.60 -1 -3 -9 856.71 47.70 1 -3 9 706.53 47.70 -1 -3 -9 752.42 47.70 1 3 9 854.91 48.90 -1 3 -9 792.52 47.90 1 3 9 688.33 48.60 1 3 9 781.22 47.20 -1 3 -9 788.22 47.90 -1 3 -9 728.33 48.80 -3 -3 -9 240.68 16.90 3 -3 9 217.98 17.50 3 -3 9 220.88 16.80 -3 -3 -9 253.57 17.00 -3 -3 -9 268.37 17.40 3 -3 9 260.77 17.00 -3 3 -9 275.57 18.40 -3 3 -9 246.58 16.90 3 3 9 246.78 16.30 3 3 9 265.87 17.90 -3 3 -9 255.87 17.00 -5 -3 -9 54.29 5.90 5 -3 9 52.29 4.90 5 -3 9 61.09 5.00 5 -3 9 46.20 5.60 -5 -3 -9 55.29 4.90 5 3 9 51.19 5.40 -5 3 -9 67.49 5.40 5 3 9 52.59 5.10 -5 3 -9 59.49 6.00 5 3 9 58.79 5.60 7 -3 9 302.57 18.80 -7 -3 -9 318.07 18.80 7 -3 9 321.07 19.20 7 -3 9 258.77 19.40 7 3 9 258.47 19.30 7 3 9 303.67 18.90 7 3 9 273.47 21.20 8 -4 -9 5.50 1.20 -8 -4 9 4.50 1.10 -8 -4 9 4.00 1.10 -8 4 9 4.10 1.20 -8 4 9 3.50 1.90 8 4 -9 5.80 2.00 -8 4 9 3.90 1.20 6 -4 -9 343.97 25.40 -6 -4 9 438.86 25.10 -6 -4 9 435.66 25.30 6 -4 -9 407.86 25.10 -6 4 9 357.16 29.10 6 4 -9 408.66 26.10 -6 4 9 341.57 25.30 -6 4 9 400.16 24.90 6 4 -9 416.16 26.10 -4 -4 9 320.97 19.20 4 -4 -9 280.17 19.90 -4 -4 9 296.27 19.20 -4 -4 9 268.37 18.80 4 -4 -9 314.67 19.20 4 4 -9 333.37 20.60 4 4 -9 302.17 19.90 -4 4 9 306.17 20.20 -4 4 9 297.17 18.90 -4 4 9 251.87 18.50 -4 4 9 249.97 19.60 2 -4 -9 107.29 7.30 -2 -4 9 80.59 7.00 -2 -4 9 77.09 6.90 -2 -4 9 81.99 6.80 2 -4 -9 86.39 7.20 2 4 -9 91.39 7.00 -2 4 9 93.09 7.90 -2 4 9 95.59 6.90 2 4 -9 94.19 8.20 2 4 -9 102.69 8.50 2 4 -9 93.29 7.60 -2 4 9 105.29 8.20 -2 4 9 91.89 6.80 0 -4 -9 28.00 3.20 0 -4 9 17.10 2.70 0 -4 9 21.20 4.50 0 -4 9 19.60 2.90 0 -4 -9 26.60 4.90 0 4 -9 20.40 3.70 0 4 9 20.90 5.30 0 4 -9 23.30 3.00 0 4 9 26.50 4.00 0 4 9 27.30 2.80 0 4 -9 25.00 4.50 2 -4 9 101.69 8.80 2 -4 9 118.39 9.30 2 -4 9 103.39 8.70 -2 -4 -9 123.49 8.70 2 -4 9 124.79 9.00 -2 -4 -9 117.19 8.70 2 -4 9 95.29 7.90 2 4 9 131.59 9.90 2 4 9 118.79 8.00 -2 4 -9 134.99 8.80 -2 4 -9 129.59 10.30 -4 -4 -9 41.20 3.80 4 -4 9 33.10 3.80 4 -4 9 34.00 4.00 -4 -4 -9 38.90 3.80 4 -4 9 34.80 3.60 4 4 9 42.30 4.40 -4 4 -9 34.30 5.00 -4 4 -9 41.80 3.50 4 4 9 40.40 4.60 6 -4 9 128.99 10.00 6 -4 9 163.98 10.10 6 -4 9 149.99 11.10 6 4 9 153.58 10.30 6 4 9 135.69 10.30 -7 -5 9 122.09 7.70 -7 -5 9 106.69 7.60 7 -5 -9 123.39 7.60 -7 5 9 106.19 7.60 -7 5 9 96.09 9.50 7 5 -9 124.99 8.40 5 -5 -9 22.30 2.50 -5 -5 9 27.40 3.10 -5 -5 9 23.30 3.10 5 5 -9 27.70 3.60 -5 5 9 23.60 2.60 5 5 -9 28.50 4.30 3 -5 -9 29.30 3.00 3 -5 -9 31.70 3.10 -3 -5 9 32.60 3.20 -3 -5 9 24.00 2.60 -3 5 9 24.80 3.40 -3 5 9 27.40 2.80 -3 5 9 20.20 3.20 3 5 -9 27.60 4.50 3 5 -9 26.90 4.10 1 -5 -9 809.32 45.70 -1 -5 9 675.43 45.40 -1 -5 9 709.83 45.20 -1 -5 9 704.63 45.40 1 -5 -9 691.93 45.30 -1 5 9 782.02 46.70 -1 5 9 736.03 46.10 1 5 -9 727.43 46.40 1 5 -9 712.33 46.60 1 -5 9 159.98 11.30 1 -5 9 168.88 11.80 -1 5 -9 190.58 13.20 1 5 9 179.28 12.50 1 5 9 153.38 12.30 3 -5 9 0.60 0.80 3 5 9 1.60 0.90 -3 5 -9 0.10 1.20 3 5 9 0.20 0.70 -3 5 -9 0.50 0.90 3 5 9 0.60 1.30 -3 5 -9 -0.30 3.00 5 -5 9 63.89 5.10 5 5 9 79.09 5.80 5 5 9 61.89 5.50 5 5 9 64.59 7.50 -4 -6 9 12.60 1.80 -4 6 9 17.40 2.80 4 6 -9 13.20 2.80 -4 6 9 11.00 3.10 4 6 -9 13.30 2.80 -4 6 9 12.60 2.10 -2 -6 9 238.18 15.70 -2 -6 9 254.27 16.20 -2 6 9 213.98 19.60 -2 6 9 257.07 17.00 2 6 -9 251.27 18.00 2 6 -9 251.97 16.60 0 -6 9 702.63 42.80 0 -6 9 598.74 42.60 0 6 -9 722.53 44.20 0 6 -9 659.53 44.40 0 6 9 751.82 44.10 2 -6 9 813.12 57.79 -2 6 -9 979.40 59.09 2 6 9 1044.10 58.69 2 6 9 1025.90 58.39 2 6 9 818.32 61.69 4 -6 9 66.19 5.00 4 6 9 68.89 5.30 4 6 9 53.39 5.70 -3 -7 9 41.30 3.40 -3 -7 9 40.40 3.30 3 7 -9 42.00 4.30 -1 -7 9 183.38 11.20 -1 7 9 156.48 11.50 1 7 -9 162.78 11.80 1 7 9 262.37 20.20 1 7 9 293.97 18.50 4 0 -10 42.70 5.10 2 0 -10 0.10 0.80 2 0 -10 4.00 1.50 -2 0 10 1.50 0.60 -2 0 10 1.40 0.80 0 0 10 162.98 12.40 0 0 -10 205.48 12.10 0 0 10 162.28 11.60 3 -1 -10 10.00 1.80 3 -1 -10 15.50 2.60 -3 -1 10 8.60 1.40 -3 1 10 8.20 2.40 3 1 -10 10.40 2.30 3 1 -10 9.80 1.70 1 -1 -10 11.70 1.90 -1 -1 10 11.30 2.80 1 -1 -10 8.20 2.10 -1 1 10 7.90 2.30 -1 1 10 11.80 1.60 -1 1 10 11.90 2.50 1 -1 10 50.89 4.10 -1 -1 -10 59.99 4.50 1 1 10 56.39 4.30 -1 1 -10 50.89 4.30 1 1 10 53.39 4.90 -1 1 -10 41.80 4.90 -2 -2 10 167.18 12.00 2 -2 -10 195.68 12.30 2 2 -10 180.38 12.90 -2 2 10 199.88 12.80 0 -2 -10 192.28 12.50 0 -2 10 177.78 11.50 0 -2 -10 166.08 11.80 0 2 10 170.48 12.10 0 2 10 172.28 12.30 0 2 -10 173.18 12.30 0 2 -10 172.28 11.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 22044 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Ni1 Ni 0.500000 0.77205(3) 0.250000 0.01638(15) Uani 1 2 d S T P . . O1 O 0.44411(8) 0.77087(8) 0.47925(14) 0.0210(3) Uani 1 1 d . . . . . O2 O 0.39806(9) 0.93729(9) 0.48467(14) 0.0270(3) Uani 1 1 d . . . . . O3 O 0.59345(8) 0.88306(9) 0.32597(16) 0.0203(3) Uani 1 1 d . . . . . H3A H 0.5838(16) 0.929(2) 0.384(3) 0.034(7) Uiso 1 1 d . . . . . H3B H 0.6010(18) 0.908(2) 0.234(4) 0.050(8) Uiso 1 1 d . . . . . N1 N 0.42254(9) 0.64631(11) 0.17068(16) 0.0184(3) Uani 1 1 d . . . . . C1 C 0.34554(11) 0.65318(13) 0.0834(2) 0.0221(3) Uani 1 1 d . . . . . H1 H 0.320774 0.720816 0.063236 0.026 Uiso 1 1 calc R U . . . C2 C 0.30060(12) 0.56591(15) 0.0215(2) 0.0266(4) Uani 1 1 d . . . . . H2 H 0.245722 0.573189 -0.038650 0.032 Uiso 1 1 calc R U . . . C3 C 0.33775(12) 0.46776(14) 0.0495(2) 0.0274(4) Uani 1 1 d . . . . . H3 H 0.308844 0.406438 0.007408 0.033 Uiso 1 1 calc R U . . . C4 C 0.41729(12) 0.45958(14) 0.1391(2) 0.0251(4) Uani 1 1 d . . . . . H4 H 0.443912 0.392853 0.158478 0.030 Uiso 1 1 calc R U . . . C5 C 0.45760(10) 0.55072(13) 0.20042(19) 0.0195(3) Uani 1 1 d . . . . . C6 C 0.40928(11) 0.84815(13) 0.5487(2) 0.0205(3) Uani 1 1 d . . . . . C7 C 0.37685(13) 0.83022(15) 0.7205(2) 0.0298(4) Uani 1 1 d . . . . . H7A H 0.322156 0.789516 0.712443 0.045 Uiso 1 1 calc R U . . . H7B H 0.365994 0.898178 0.772859 0.045 Uiso 1 1 calc R U . . . H7C H 0.421422 0.791370 0.787378 0.045 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 Ni1 0.0208(2) 0.0148(2) 0.0138(2) 0.000 0.00338(14) 0.000 O1 0.0287(6) 0.0178(6) 0.0172(6) 0.0010(4) 0.0072(5) 0.0025(4) O2 0.0425(7) 0.0196(6) 0.0192(6) -0.0006(5) 0.0051(5) 0.0066(5) O3 0.0270(6) 0.0178(6) 0.0163(6) -0.0014(5) 0.0029(4) -0.0017(4) N1 0.0214(6) 0.0179(6) 0.0164(6) -0.0003(5) 0.0057(5) -0.0010(5) C1 0.0237(8) 0.0230(8) 0.0198(8) -0.0016(6) 0.0051(6) -0.0011(6) C2 0.0255(8) 0.0312(9) 0.0234(8) -0.0033(7) 0.0039(6) -0.0045(7) C3 0.0311(9) 0.0249(9) 0.0269(9) -0.0074(7) 0.0076(7) -0.0087(7) C4 0.0315(9) 0.0185(8) 0.0261(8) -0.0031(7) 0.0093(7) -0.0025(7) C5 0.0245(8) 0.0175(8) 0.0173(7) -0.0007(6) 0.0085(6) -0.0011(6) C6 0.0231(8) 0.0214(8) 0.0172(7) -0.0012(6) 0.0037(6) 0.0003(6) C7 0.0412(10) 0.0283(9) 0.0210(8) 0.0004(7) 0.0128(7) 0.0047(8) 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' Ni Ni -3.0029 0.5091 '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' 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 N1 Ni1 N1 78.84(8) . 2_655 ? N1 Ni1 O3 171.44(5) . . ? N1 Ni1 O3 93.55(5) 2_655 . ? N1 Ni1 O3 93.55(5) . 2_655 ? N1 Ni1 O3 171.44(5) 2_655 2_655 ? O3 Ni1 O3 94.29(7) . 2_655 ? N1 Ni1 O1 88.30(5) . 2_655 ? N1 Ni1 O1 91.06(5) 2_655 2_655 ? O3 Ni1 O1 87.92(5) . 2_655 ? O3 Ni1 O1 92.64(5) 2_655 2_655 ? N1 Ni1 O1 91.06(5) . . ? N1 Ni1 O1 88.30(5) 2_655 . ? O3 Ni1 O1 92.64(5) . . ? O3 Ni1 O1 87.92(5) 2_655 . ? O1 Ni1 O1 179.18(6) 2_655 . ? C6 O1 Ni1 126.27(10) . . ? Ni1 O3 H3A 123.3(19) . . ? Ni1 O3 H3B 97(2) . . ? H3A O3 H3B 107(3) . . ? C1 N1 C5 118.82(14) . . ? C1 N1 Ni1 125.64(11) . . ? C5 N1 Ni1 115.34(11) . . ? N1 C1 C2 122.80(16) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.23(16) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 119.55(16) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.88(16) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.69(15) . . ? N1 C5 C5 115.04(9) . 2_655 ? C4 C5 C5 123.26(10) . 2_655 ? O2 C6 O1 124.84(15) . . ? O2 C6 C7 118.08(15) . . ? O1 C6 C7 117.05(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 Ni1 N1 2.0697(14) . ? Ni1 N1 2.0697(14) 2_655 ? Ni1 O3 2.0755(12) . ? Ni1 O3 2.0755(12) 2_655 ? Ni1 O1 2.0790(11) 2_655 ? Ni1 O1 2.0791(11) . ? O1 C6 1.2621(19) . ? O2 C6 1.254(2) . ? O3 H3A 0.77(3) . ? O3 H3B 0.82(3) . ? N1 C1 1.341(2) . ? N1 C5 1.344(2) . ? C1 C2 1.385(2) . ? C1 H1 0.9500 . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(2) . ? C4 H4 0.9500 . ? C5 C5 1.486(3) 2_655 ? C6 C7 1.516(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 C5 N1 C1 C2 -0.4(2) . . . . ? Ni1 N1 C1 C2 174.12(12) . . . . ? N1 C1 C2 C3 -0.9(3) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C1 N1 C5 C4 1.8(2) . . . . ? Ni1 N1 C5 C4 -173.23(12) . . . . ? C1 N1 C5 C5 -179.32(15) . . . 2_655 ? Ni1 N1 C5 C5 5.6(2) . . . 2_655 ? C3 C4 C5 N1 -1.9(2) . . . . ? C3 C4 C5 C5 179.31(18) . . . 2_655 ? Ni1 O1 C6 O2 4.7(2) . . . . ? Ni1 O1 C6 C7 -176.91(12) . . . . ?