#------------------------------------------------------------------------------ #$Date: 2022-11-08 19:23:43 +0000 (Tue, 08 Nov 2022) $ #$Revision: 279108 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244208.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2244208 loop_ _publ_author_name 'Krebs, Christoph' 'Jess, Inke' 'N\"ather, Christian' _publ_section_title ; Syntheses and crystal structures of the ethanol, acetonitrile and diethyl ether Werner clathrates bis(isothiocyanato-\kN)tetrakis(3-methylpyridine-\kN)nickel(II) ; _journal_coeditor_code HB8036 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 993 _journal_page_last 998 _journal_paper_doi 10.1107/S2056989022008891 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac '[Ni (N C S )2 (C6 H7 N )4], 2C2 H3 N' _chemical_formula_moiety 'C26 H28 N6 Ni S2, 2(C2 H3 N)' _chemical_formula_sum 'C30 H34 N8 Ni S2' _chemical_formula_weight 629.48 _chemical_name_systematic ; Bis(isothiocyanato-\kN)tetrakis(3-methylpyridine-\kN)\ nickel(II) acetonitrile disolvate ; _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 geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214) ; _cell_angle_alpha 90 _cell_angle_beta 96.8250(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.79900(10) _cell_length_b 11.30330(10) _cell_length_c 15.86390(10) _cell_measurement_reflns_used 26840 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 79.1620 _cell_measurement_theta_min 4.5430 _cell_volume 3347.04(4) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2021) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 1999) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _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 0.0205 _diffrn_reflns_av_unetI/netI 0.0072 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 35196 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.668 _diffrn_reflns_theta_min 4.573 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.247 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour 'light purple' _exptl_crystal_density_diffrn 1.249 _exptl_crystal_description block _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.799 _refine_diff_density_min -0.461 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 3605 _refine_ls_number_restraints 82 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0456 _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^)+(0.0965P)^2^+2.6920P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1517 _refine_ls_wR_factor_ref 0.1526 _reflns_number_gt 3462 _reflns_number_total 3605 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8036sup1.cif _cod_data_source_block 2 _cod_database_code 2244208 _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 0.603 _shelx_estimated_absorpt_t_max 0.896 _shelx_hkl_file ; 0 0 -1 0.01 0.04 0 0 1 0.02 0.04 0 0 1 0.00 0.04 0 0 -2 1012.25 6.95 0 0 2 987.11 6.94 0 0 -3 0.06 0.14 0 0 3 -0.01 0.10 0 0 -3 0.02 0.11 0 0 3 0.14 0.14 0 0 4 4579.09 31.76 0 0 4 4601.98 31.67 0 0 4 4605.32 31.91 0 0 -4 4601.59 31.75 0 0 -5 0.05 0.16 0 0 5 0.07 0.17 0 0 5 1.23 0.18 0 0 -5 0.14 0.16 0 0 5 1.31 0.24 0 0 6 354.08 3.40 0 0 6 345.53 3.26 0 0 -6 369.77 3.46 0 0 -6 358.51 3.29 0 0 6 359.29 3.61 0 0 -7 0.05 0.17 0 0 7 0.03 0.15 0 0 7 0.13 0.18 0 0 -7 0.03 0.19 0 0 7 -0.01 0.21 0 0 -8 133.91 1.85 0 0 8 134.29 1.96 0 0 8 127.37 2.12 0 0 -8 132.76 1.96 0 0 -9 -0.03 0.17 0 0 9 0.09 0.20 0 0 9 0.07 0.25 0 0 -9 0.01 0.20 0 0 9 0.29 0.26 0 0 10 147.38 1.47 0 0 10 145.43 2.57 0 0 10 140.36 2.56 0 0 -10 148.74 2.36 0 0 -10 140.88 1.42 0 0 10 150.95 1.54 0 0 -10 154.46 1.51 0 0 -10 143.47 2.11 0 0 10 145.44 2.29 0 0 -11 0.45 0.28 0 0 11 0.02 0.31 0 0 11 0.01 0.24 0 0 -11 0.26 0.17 0 0 11 0.15 0.18 0 0 11 -0.03 0.15 0 0 -12 427.95 5.11 0 0 12 430.12 5.56 0 0 -12 430.17 5.54 0 0 -12 462.21 3.77 0 0 12 461.56 3.84 0 0 -12 449.26 3.68 0 0 12 455.75 3.71 0 0 13 0.08 0.18 0 0 -13 0.01 0.18 0 0 13 0.02 0.37 0 0 -13 0.08 0.33 0 0 13 0.12 0.22 0 0 -13 -0.11 0.21 0 0 -13 0.00 0.19 0 0 -13 0.05 0.18 0 0 14 221.78 2.14 0 0 -14 220.55 2.14 0 0 14 212.88 3.86 0 0 -14 218.91 3.80 0 0 -14 212.62 2.19 0 0 14 224.22 2.29 0 0 -14 223.29 2.23 0 0 -14 218.71 2.25 0 0 -14 221.36 2.22 0 0 -15 -0.03 0.17 0 0 -15 0.11 0.20 0 0 -15 0.11 0.21 0 0 15 -0.04 0.24 0 0 15 -0.06 0.17 0 0 -15 0.12 0.20 0 0 -15 0.01 0.19 0 0 -16 0.16 0.17 0 0 16 0.33 0.22 0 0 -16 0.39 0.18 0 0 16 0.45 0.16 0 0 17 -0.02 0.14 0 0 -17 0.00 0.17 0 0 17 -0.11 0.19 0 0 17 -0.02 0.19 0 0 -17 0.07 0.13 0 0 -17 -0.08 0.18 0 0 -17 -0.04 0.15 0 0 18 1.05 0.17 0 0 18 1.22 0.18 0 0 -18 1.25 0.17 0 0 19 0.00 0.11 0 0 -19 0.01 0.11 0 0 -19 0.03 0.10 0 0 -20 11.41 0.19 0 -2 0 61.89 0.78 0 2 0 62.12 0.71 0 2 0 57.22 0.84 0 -2 0 57.04 0.58 0 -2 1 119.33 1.29 0 2 1 119.90 1.26 0 -2 -1 116.99 1.35 0 2 -1 117.24 1.30 0 -2 1 116.40 1.08 0 2 1 117.90 1.34 0 -2 2 1619.49 11.17 0 2 -2 1516.79 11.16 0 2 2 1509.40 11.18 0 -2 -2 1629.52 11.34 0 2 -2 1587.31 11.11 0 2 2 1495.34 11.22 0 -2 2 1505.42 10.74 0 2 -3 78.24 1.13 0 -2 3 78.03 1.13 0 -2 -3 79.22 1.23 0 2 -3 80.63 1.08 0 2 3 80.17 1.20 0 2 3 77.50 1.18 0 -2 4 9.48 0.43 0 2 -4 9.73 0.42 0 2 -4 9.60 0.44 0 -2 -4 10.78 0.50 0 2 -4 9.61 0.38 0 2 4 11.05 0.48 0 2 4 11.32 0.49 0 2 -5 501.10 4.43 0 -2 -5 496.30 4.52 0 -2 5 487.88 4.48 0 2 5 468.49 4.60 0 -2 -5 473.39 4.59 0 2 -5 499.91 4.21 0 -2 5 495.17 3.93 0 2 5 496.03 4.53 0 2 5 505.86 4.52 0 -2 -6 81.88 1.44 0 -2 6 78.83 1.45 0 2 -6 80.41 1.38 0 2 6 77.46 1.51 0 2 -6 77.52 1.23 0 2 6 76.48 1.42 0 -2 6 76.62 1.07 0 -2 7 26.90 0.91 0 -2 -7 26.88 0.85 0 2 7 25.87 0.94 0 2 -7 27.74 0.83 0 2 -7 26.62 0.72 0 2 7 26.00 0.85 0 -2 7 25.43 0.63 0 2 8 1444.79 12.39 0 -2 -8 1492.75 11.99 0 -2 8 1474.81 12.22 0 2 -8 1477.16 11.89 0 -2 8 1542.05 11.29 0 2 8 1532.40 12.22 0 2 8 1538.83 12.05 0 2 -8 1472.66 11.49 0 2 9 132.19 1.37 0 2 -9 128.62 1.30 0 2 -9 127.21 2.16 0 -2 9 127.78 2.36 0 2 9 126.28 2.45 0 -2 -9 126.15 2.16 0 2 -9 136.22 1.35 0 -2 -9 129.96 1.35 0 2 9 125.83 1.28 0 2 -9 122.67 1.87 0 2 9 131.48 2.20 0 2 9 133.52 2.34 0 2 10 23.82 0.52 0 -2 -10 23.77 0.47 0 2 10 23.52 0.49 0 2 -10 23.23 0.48 0 -2 -10 23.80 0.94 0 -2 -10 23.27 0.88 0 2 -10 21.70 0.91 0 2 10 22.76 1.07 0 -2 10 22.24 1.03 0 2 -10 23.53 0.45 0 -2 -10 23.98 0.50 0 2 10 23.65 0.48 0 -2 10 22.95 0.51 0 -2 -10 24.55 0.52 0 2 -10 24.34 0.51 0 2 10 23.60 0.94 0 2 10 25.79 1.05 0 -2 -11 67.02 0.89 0 2 -11 65.56 0.90 0 2 11 66.14 0.89 0 2 -11 65.76 1.79 0 -2 -11 62.61 1.52 0 2 11 62.91 1.86 0 -2 -11 63.36 1.63 0 2 -11 64.17 1.63 0 2 11 60.67 1.72 0 2 11 67.19 0.96 0 2 11 65.77 0.87 0 2 -11 66.73 0.95 0 -2 -11 66.84 0.95 0 -2 11 66.72 0.95 0 2 -11 65.01 1.65 0 2 11 70.77 1.81 0 2 12 69.16 1.86 0 -2 -12 67.57 2.05 0 2 -12 66.70 1.76 0 2 12 82.34 1.12 0 2 -12 79.21 1.05 0 2 12 79.53 1.01 0 -2 -12 80.76 1.03 0 2 12 73.63 2.00 0 -2 -12 72.29 1.81 0 2 -12 74.92 2.01 0 2 -12 74.20 1.82 0 2 12 77.55 2.17 0 2 12 71.10 0.96 0 -2 -12 70.62 1.07 0 -2 -12 71.61 1.07 0 2 12 83.91 1.14 0 -2 12 86.14 1.12 0 -2 -12 88.34 1.13 0 -2 -13 2.85 0.56 0 2 13 3.16 0.49 0 2 13 4.23 0.31 0 -2 -13 4.05 0.26 0 2 13 3.78 0.24 0 2 -13 3.58 0.27 0 2 13 3.42 0.55 0 2 -13 3.93 0.54 0 2 13 3.44 0.23 0 2 -13 3.13 0.26 0 -2 -13 3.51 0.29 0 -2 13 4.61 0.31 0 -2 -13 4.71 0.31 0 2 -13 4.32 0.33 0 2 -13 3.60 0.25 0 -2 -13 3.53 0.29 0 2 14 356.69 3.16 0 2 -14 354.52 3.07 0 -2 -14 355.76 3.05 0 2 -14 344.65 3.28 0 2 -14 347.80 3.11 0 -2 -14 348.52 3.13 0 -2 14 350.47 3.15 0 2 -14 348.22 3.04 0 -2 -14 345.93 3.16 0 2 -14 357.59 3.11 0 -2 -14 350.12 3.11 0 -2 15 0.30 0.24 0 2 15 0.47 0.21 0 -2 -15 0.43 0.18 0 2 -15 0.50 0.18 0 2 -15 0.27 0.23 0 2 -15 0.66 0.19 0 -2 -15 0.45 0.21 0 -2 15 0.58 0.22 0 -2 -15 0.48 0.21 0 2 -15 0.53 0.20 0 2 -15 0.66 0.17 0 -2 -15 0.51 0.21 0 2 -16 76.14 0.99 0 -2 -16 73.10 0.97 0 -2 16 76.52 1.11 0 -2 -16 71.34 1.04 0 2 16 75.51 1.04 0 -2 -16 74.57 1.06 0 -2 16 74.20 1.05 0 2 -16 80.68 1.04 0 -2 -16 80.69 1.06 0 -2 -16 78.47 1.07 0 -2 -17 0.06 0.16 0 2 -17 0.14 0.16 0 2 17 0.04 0.16 0 -2 -17 0.05 0.18 0 2 -17 0.10 0.13 0 -2 17 0.00 0.17 0 -2 17 0.04 0.19 0 2 17 0.05 0.16 0 2 -17 0.07 0.15 0 -2 -17 0.15 0.17 0 -2 -18 0.81 0.15 0 2 -18 0.41 0.14 0 2 18 0.52 0.13 0 -2 -18 0.45 0.14 0 -2 18 0.28 0.14 0 2 -18 0.97 0.15 0 -2 -18 1.00 0.16 0 2 18 0.44 0.13 0 -2 18 0.88 0.15 0 2 18 1.01 0.15 0 2 -19 6.15 0.19 0 -2 -19 6.78 0.20 0 4 0 2150.69 15.59 0 4 0 2130.15 15.02 0 -4 1 90.09 1.14 0 -4 -1 88.57 1.07 0 -4 -1 91.77 1.53 0 -4 1 90.67 1.40 0 4 -1 89.62 1.11 0 4 1 89.45 1.29 0 -4 -2 205.75 1.64 0 4 -2 207.63 1.74 0 4 2 226.11 2.49 0 4 2 224.45 2.02 0 4 -2 231.25 2.00 0 -4 2 235.63 2.53 0 -4 -2 224.08 2.70 0 4 -2 229.51 2.60 0 -4 2 216.49 2.03 0 -4 -2 216.93 2.17 0 4 2 225.45 2.68 0 -4 3 470.97 4.37 0 4 3 468.42 4.46 0 4 -3 464.62 4.41 0 -4 -3 467.24 4.65 0 -4 3 481.02 3.73 0 -4 -3 451.08 4.10 0 4 3 484.45 4.66 0 -4 4 25.36 0.78 0 4 4 25.90 0.86 0 4 -4 24.55 0.82 0 -4 -4 24.34 0.88 0 4 -4 24.83 0.77 0 4 4 18.85 0.77 0 4 4 18.86 0.76 0 -4 5 52.05 1.22 0 4 5 53.04 1.33 0 4 -5 57.32 1.30 0 -4 -5 51.96 1.35 0 4 -5 52.42 1.15 0 4 5 51.53 1.30 0 4 5 54.24 1.35 0 -4 6 974.21 8.48 0 4 -6 976.53 8.44 0 4 6 975.15 8.72 0 4 -6 976.16 8.09 0 -4 -6 967.17 8.78 0 4 6 962.04 8.65 0 4 6 975.92 8.62 0 4 7 4.02 0.48 0 -4 -7 4.45 0.47 0 -4 7 4.25 0.46 0 4 -7 4.23 0.46 0 4 7 4.81 0.50 0 -4 -7 3.70 0.47 0 4 -7 4.16 0.37 0 4 8 1147.81 8.40 0 4 8 1148.68 8.40 0 4 8 1162.50 8.36 0 4 -8 1129.96 8.31 0 4 8 1125.33 10.41 0 -4 -8 1134.48 10.19 0 -4 8 1152.84 10.29 0 4 -8 1148.49 10.10 0 4 8 1152.31 8.35 0 4 -8 1123.96 9.43 0 4 8 1191.61 10.38 0 -4 -8 1184.87 8.44 0 4 9 1.97 0.22 0 4 9 1.82 0.20 0 4 -9 2.21 0.20 0 4 9 1.99 0.21 0 4 -9 1.75 0.37 0 -4 9 2.19 0.47 0 -4 -9 1.47 0.36 0 4 9 1.74 0.41 0 -4 -9 2.11 0.40 0 4 9 1.99 0.43 0 4 9 2.04 0.19 0 4 -9 1.69 0.17 0 -4 -9 1.91 0.20 0 -4 -9 2.03 0.22 0 -4 -10 50.70 0.83 0 4 10 48.40 0.80 0 4 10 48.74 0.76 0 4 -10 50.44 0.78 0 4 -10 46.79 1.50 0 -4 -10 46.35 1.48 0 -4 10 48.23 1.62 0 4 -10 48.70 0.73 0 -4 -10 50.89 0.80 0 -4 10 49.33 0.74 0 -4 -10 43.50 1.51 0 4 10 46.85 1.53 0 4 10 46.08 1.58 0 4 10 45.06 0.76 0 4 -11 68.53 0.91 0 -4 -11 72.07 0.99 0 -4 11 70.33 1.03 0 -4 -11 65.25 0.98 0 -4 -11 68.84 0.95 0 4 11 70.19 1.01 0 4 -11 67.10 0.97 0 4 11 68.36 0.94 0 4 -11 63.84 1.84 0 -4 11 66.71 2.02 0 -4 -11 65.62 1.80 0 4 11 67.47 2.06 0 -4 -11 72.06 1.04 0 -4 11 70.27 0.95 0 4 11 67.59 0.97 0 -4 -11 65.70 1.95 0 4 11 68.68 1.90 0 4 11 66.44 1.97 0 4 -12 25.35 0.71 0 4 12 29.09 0.62 0 -4 12 24.99 0.62 0 -4 -12 26.29 0.59 0 4 12 26.34 0.63 0 -4 -12 26.42 0.58 0 4 -12 29.38 0.62 0 4 12 27.17 0.61 0 4 -12 27.20 1.22 0 4 -12 24.90 1.36 0 4 12 27.10 1.35 0 -4 -12 24.12 1.12 0 -4 12 25.96 1.31 0 4 12 24.57 1.14 0 -4 -12 27.70 0.56 0 4 12 31.42 1.36 0 4 -12 28.58 0.56 0 -4 -12 29.85 1.38 0 4 12 29.23 1.26 0 -4 -12 27.36 0.62 0 -4 -12 25.41 0.62 0 -4 12 25.96 0.56 0 4 12 25.51 0.62 0 -4 -13 2.56 0.27 0 -4 13 2.67 0.24 0 4 13 2.53 0.28 0 4 13 2.53 0.29 0 -4 -13 2.40 0.24 0 4 -13 2.46 0.24 0 4 13 2.60 0.25 0 4 -13 2.25 0.33 0 4 13 2.79 0.24 0 -4 13 2.46 0.28 0 -4 -13 2.84 0.23 0 4 -13 2.96 0.23 0 -4 -13 2.57 0.26 0 -4 -14 64.46 0.99 0 4 14 64.67 1.03 0 -4 14 65.20 0.93 0 4 14 68.53 1.05 0 4 -14 63.78 0.96 0 -4 -14 65.20 0.93 0 4 14 64.64 0.96 0 4 -14 65.47 1.15 0 4 14 68.09 0.95 0 -4 14 66.36 1.03 0 4 -14 67.29 0.91 0 -4 -14 65.86 0.92 0 -4 -14 60.92 0.97 0 -4 15 2.12 0.26 0 -4 -15 1.98 0.24 0 4 15 2.03 0.25 0 4 15 2.27 0.21 0 4 -15 1.95 0.22 0 -4 -15 2.01 0.20 0 4 -15 1.85 0.30 0 4 15 2.33 0.21 0 4 15 2.20 0.25 0 -4 -15 1.72 0.22 0 -4 15 2.18 0.21 0 -4 -15 2.10 0.20 0 4 -15 2.26 0.21 0 -4 -16 23.05 0.53 0 4 16 23.04 0.54 0 -4 -16 23.01 0.47 0 4 -16 23.29 0.49 0 4 16 23.08 0.46 0 4 16 22.72 0.54 0 -4 -16 22.11 0.51 0 -4 16 23.45 0.54 0 4 -16 21.97 0.59 0 4 16 26.51 0.52 0 -4 -16 25.66 0.49 0 4 -16 25.98 0.48 0 -4 -17 1.15 0.15 0 4 17 1.29 0.19 0 -4 -17 1.28 0.17 0 -4 17 1.32 0.18 0 4 -17 1.17 0.19 0 -4 -17 1.40 0.18 0 4 17 1.38 0.18 0 -4 17 1.12 0.14 0 -4 -18 1.30 0.15 0 -4 18 1.85 0.15 0 4 18 1.67 0.15 0 -4 -18 0.84 0.10 0 4 -18 1.29 0.13 0 -4 -18 1.57 0.15 0 4 18 1.39 0.14 0 4 -19 5.56 0.17 0 -4 -19 6.61 0.16 0 -6 0 2651.05 19.01 0 6 0 2523.98 20.04 0 -6 0 2672.55 20.26 0 6 0 2537.46 18.83 0 -6 0 2706.15 19.63 0 6 0 2616.14 19.47 0 -6 1 2.57 0.25 0 6 -1 3.31 0.42 0 6 1 3.17 0.43 0 -6 -1 3.00 0.45 0 6 1 2.91 0.30 0 6 1 2.70 0.29 0 -6 1 2.87 0.37 0 6 2 285.95 3.71 0 6 -2 285.50 3.64 0 -6 -2 285.50 3.84 0 6 2 288.02 3.31 0 -6 2 293.66 3.52 0 -6 -3 45.91 0.98 0 6 3 45.07 1.39 0 6 3 45.52 1.42 0 6 -3 46.64 1.30 0 -6 -3 50.75 1.51 0 6 -3 46.35 1.41 0 -6 3 53.43 1.35 0 6 3 50.60 1.28 0 -6 -4 162.29 1.65 0 -6 -4 168.29 2.97 0 6 4 161.74 1.66 0 6 4 165.83 2.62 0 -6 4 172.64 2.61 0 6 -4 165.44 2.79 0 6 4 176.52 2.95 0 6 4 163.68 2.84 0 6 -4 172.03 2.62 0 -6 -4 174.81 2.26 0 6 -4 151.82 1.60 0 6 -5 42.09 0.70 0 -6 -5 43.73 0.73 0 -6 -5 40.83 1.43 0 6 5 39.45 0.65 0 6 -5 41.24 0.67 0 6 5 42.80 0.70 0 6 -5 38.57 1.31 0 6 5 39.25 1.28 0 -6 5 40.68 1.23 0 6 5 41.42 0.72 0 -6 -5 40.02 1.08 0 6 5 39.70 1.39 0 6 6 162.79 1.67 0 -6 -6 158.57 1.60 0 6 -6 160.39 1.61 0 6 6 157.49 1.59 0 6 6 153.07 1.56 0 6 -6 151.98 1.59 0 6 6 158.75 1.64 0 6 6 156.76 2.80 0 -6 6 154.83 2.66 0 6 -6 156.20 2.80 0 6 6 148.95 1.58 0 -6 -6 148.91 2.91 0 -6 -6 159.85 1.68 0 -6 -6 149.27 2.40 0 6 6 150.16 2.91 0 6 6 154.88 2.90 0 -6 -7 11.45 0.37 0 6 -7 11.05 0.37 0 -6 7 10.83 0.32 0 6 7 11.27 0.36 0 6 7 11.16 0.37 0 6 -7 12.75 0.39 0 6 7 10.38 0.39 0 6 7 10.96 0.39 0 6 7 10.28 0.76 0 -6 7 10.98 0.73 0 6 -7 11.13 0.76 0 6 7 10.55 0.36 0 -6 -7 10.85 0.84 0 6 7 10.59 0.80 0 -6 -7 11.03 0.68 0 6 7 10.21 0.79 0 -6 -7 11.16 0.40 0 -6 -8 229.97 2.17 0 6 -8 232.48 2.18 0 -6 8 226.93 2.08 0 6 8 231.45 2.21 0 6 -8 226.05 2.17 0 6 8 230.33 2.24 0 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1.27 2 2 8 0.19 0.24 -2 2 -8 0.65 0.22 -2 2 -8 0.45 0.19 -2 -2 -8 0.29 0.21 2 -2 8 0.50 0.30 2 2 8 0.33 0.29 -2 2 -8 0.72 0.24 -2 -2 -8 0.30 0.26 -2 -2 -9 107.83 1.20 2 -2 9 102.43 1.14 2 2 9 104.76 1.20 -2 2 -9 102.09 1.15 -2 -2 -9 104.50 1.15 2 2 9 104.83 1.14 -2 2 -9 103.03 1.96 -2 2 -9 101.90 1.77 -2 2 -9 104.93 2.21 -2 -2 -9 102.98 1.81 2 2 9 103.66 2.22 2 -2 9 104.22 2.14 -2 -2 -9 105.55 1.20 2 2 9 100.06 1.10 -2 2 -9 99.61 1.84 2 2 9 105.26 1.92 2 2 9 103.06 2.06 -2 -2 -9 105.46 2.19 2 -2 10 294.59 2.56 -2 -2 -10 304.44 2.62 -2 -2 -10 291.55 2.55 -2 2 -10 293.65 2.56 2 2 10 292.76 2.61 -2 -2 -10 292.13 2.45 -2 2 -10 293.69 2.49 2 2 10 292.90 2.52 2 -2 10 285.57 4.06 2 2 10 291.67 4.22 -2 2 -10 274.50 3.42 -2 2 -10 291.77 3.83 -2 -2 -10 282.88 3.49 -2 2 -10 281.05 4.16 -2 -2 -10 301.19 2.62 2 2 10 289.83 2.48 -2 -2 -10 280.11 4.05 2 2 10 300.47 3.98 2 2 10 292.31 3.66 -2 2 -10 291.74 3.68 -2 -2 -10 299.52 4.21 -2 2 -11 0.58 0.19 2 -2 11 0.88 0.20 -2 -2 -11 0.59 0.19 -2 -2 -11 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34.28 0.70 2 12 -2 33.22 0.70 -2 12 2 34.70 0.74 -2 -12 1 2.60 0.19 2 12 -1 2.99 0.20 -2 12 1 2.70 0.23 -2 -12 1 2.43 0.26 2 12 -1 2.46 0.26 -2 -12 1 2.03 0.28 -2 12 1 2.14 0.28 2 -12 -1 2.13 0.28 2 12 -1 2.15 0.29 2 -12 0 1.81 0.27 -2 12 0 1.68 0.27 -2 -12 0 2.11 0.19 2 12 0 2.24 0.19 -2 12 0 2.18 0.22 2 12 0 1.84 0.26 -2 -12 0 1.87 0.28 -2 -12 0 1.54 0.24 2 12 0 2.26 0.28 -2 12 0 1.87 0.27 -2 12 -1 1.26 0.24 2 12 1 1.46 0.26 2 12 1 1.23 0.20 2 12 1 1.57 0.27 -2 -12 -1 1.08 0.18 -2 -12 -1 1.55 0.24 -2 12 -1 1.01 0.20 -2 12 -1 1.04 0.19 2 12 1 1.43 0.26 -2 -12 -1 1.22 0.26 2 -12 1 1.30 0.25 2 12 2 333.61 2.90 -2 -12 -2 326.17 3.09 -2 12 -2 334.22 3.02 2 12 2 336.19 3.01 -2 -12 -2 334.17 2.78 -2 -12 -2 329.35 2.97 -2 12 -2 340.39 2.85 -2 12 -2 341.50 2.82 -2 12 -2 334.99 3.01 2 12 2 328.80 3.06 2 12 3 3.39 0.31 2 12 3 3.42 0.29 -2 12 -3 3.53 0.27 2 12 3 3.63 0.26 2 12 3 3.53 0.29 -2 -12 -3 3.25 0.30 -2 12 -3 3.59 0.30 -2 -12 -3 3.44 0.23 -2 -12 -3 3.24 0.26 -2 12 -3 3.60 0.24 -2 12 -3 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1.62 0.49 -8 -8 5 1.87 0.28 8 8 -5 2.47 0.24 -8 -8 4 188.15 2.07 8 8 -4 190.45 2.03 -8 -8 4 188.08 1.99 -8 8 4 186.72 2.07 -8 -8 4 184.39 2.06 -8 8 4 183.77 1.95 8 -8 -4 183.41 3.65 -8 8 4 184.35 1.91 -8 8 4 188.22 1.93 -8 -8 4 183.48 1.91 -8 8 4 185.56 1.85 -8 -8 4 194.65 1.95 -8 8 4 181.18 1.93 -8 8 4 187.41 1.98 8 8 -4 185.54 1.89 -8 -8 3 65.27 1.10 8 8 -3 67.66 1.11 8 8 -3 67.66 1.07 -8 -8 3 67.08 1.04 -8 8 3 67.01 1.08 -8 -8 3 66.45 1.10 -8 8 3 68.38 1.04 8 -8 -3 64.57 2.06 -8 8 3 67.10 0.98 -8 8 3 66.78 0.98 -8 -8 3 66.93 0.98 -8 8 3 65.60 0.93 -8 -8 3 62.96 1.96 8 8 -3 69.87 2.19 -8 -8 3 67.74 1.78 -8 8 3 62.09 1.01 -8 8 3 67.26 1.02 8 8 -2 304.49 2.86 -8 -8 2 304.13 2.84 -8 8 2 303.68 2.87 -8 -8 2 313.83 2.95 8 8 -2 290.70 4.82 -8 -8 2 311.57 4.22 8 8 -2 269.34 4.23 -8 8 2 304.02 2.68 -8 8 2 292.79 2.71 -8 8 2 299.25 2.65 -8 -8 2 303.12 2.73 -8 -8 2 281.46 4.50 8 8 -2 306.49 2.96 -8 -8 2 300.53 2.94 -8 8 2 292.00 2.84 -8 8 2 306.18 2.79 -8 -8 1 67.49 1.13 8 8 -1 68.79 1.13 8 8 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4 94.76 1.36 8 8 5 2.89 0.28 -8 -8 -5 3.00 0.30 8 8 5 2.62 0.33 8 8 5 2.80 0.31 -8 -8 -5 2.47 0.31 -8 8 -5 2.94 0.28 -8 -8 -5 3.11 0.30 -8 8 -5 3.22 0.32 -8 8 -5 2.83 0.26 8 8 5 3.13 0.26 -8 8 -5 3.15 0.28 -8 -8 -5 2.60 0.26 -8 -8 -6 195.00 2.17 8 8 6 200.20 2.18 -8 -8 -6 195.21 2.23 -8 8 -6 192.00 2.15 -8 -8 -6 185.93 2.10 -8 8 -6 191.82 1.97 -8 8 -6 191.05 2.00 8 8 6 205.01 1.98 -8 8 -6 197.63 2.06 -8 -8 -6 192.61 1.99 -8 8 -6 189.93 2.12 8 8 7 1.46 0.28 -8 -8 -7 1.96 0.28 8 8 7 1.26 0.27 -8 -8 -7 1.52 0.31 -8 8 -7 1.71 0.30 -8 8 -7 1.90 0.27 -8 8 -7 1.80 0.25 -8 -8 -7 1.77 0.27 8 8 7 1.79 0.24 -8 8 -7 1.58 0.21 -8 8 -7 1.67 0.26 -8 -8 -7 1.75 0.24 -8 8 -7 1.74 0.27 8 8 8 212.73 2.28 8 8 8 216.97 2.36 8 8 8 224.85 2.30 -8 -8 -8 222.11 2.35 -8 8 -8 219.72 2.26 -8 8 -8 215.19 2.17 -8 -8 -8 213.82 2.26 8 8 8 227.99 2.13 -8 8 -8 217.29 2.15 -8 8 -8 222.29 2.21 -8 8 -8 220.75 2.29 -8 -8 -8 216.29 2.13 -8 -8 -9 0.30 0.21 8 8 9 0.12 0.25 8 8 9 0.44 0.27 8 8 9 0.21 0.21 8 8 9 0.17 0.21 -8 -8 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1.69 0.18 -8 -10 7 1.64 0.24 8 10 -7 1.62 0.21 -8 -10 7 1.35 0.25 8 10 -7 1.17 0.25 8 -10 -7 1.54 0.21 8 10 -6 1.11 0.25 -8 -10 6 1.24 0.25 8 -10 -6 1.10 0.22 -8 -10 6 1.57 0.25 -8 10 6 1.66 0.21 -8 10 6 2.12 0.23 -8 10 6 1.58 0.24 8 10 -6 0.85 0.21 -8 10 6 1.42 0.18 -8 -10 6 1.44 0.23 8 10 -6 1.24 0.27 8 10 -6 1.49 0.21 8 10 -5 0.67 0.24 -8 -10 5 0.76 0.24 8 -10 -5 0.77 0.21 -8 -10 5 0.93 0.25 -8 10 5 1.61 0.22 -8 10 5 1.54 0.21 -8 10 5 0.98 0.23 -8 -10 5 1.01 0.22 -8 10 5 1.13 0.18 8 10 -5 0.88 0.26 8 10 -5 1.13 0.20 -8 -10 4 12.58 0.47 -8 -10 4 12.47 0.49 8 10 -4 12.24 0.38 -8 10 4 12.66 0.42 -8 10 4 12.63 0.41 -8 10 4 12.78 0.43 -8 10 4 13.23 0.46 -8 10 4 11.86 0.36 -8 -10 4 13.25 0.44 8 10 -4 12.23 0.40 -8 10 4 12.62 0.40 8 10 -4 13.02 0.48 8 10 -3 0.31 0.22 -8 10 3 0.02 0.23 -8 -10 3 0.19 0.23 -8 10 3 0.15 0.20 8 10 -3 0.11 0.16 -8 10 3 0.27 0.17 -8 10 3 0.16 0.21 -8 10 3 0.36 0.21 -8 -10 3 0.10 0.20 -8 10 3 0.16 0.16 -8 -10 3 0.09 0.20 8 10 -3 -0.06 0.25 8 10 -3 0.14 0.18 -8 10 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1.02 -8 -10 -6 68.95 0.94 -8 -10 -6 66.36 1.07 -8 10 -6 69.60 0.98 -8 10 -6 68.90 1.05 -8 -10 -7 0.02 0.18 8 10 7 -0.07 0.20 8 10 7 -0.12 0.20 -8 10 -7 -0.01 0.21 -8 -10 -7 -0.01 0.17 -8 -10 -7 0.00 0.21 -8 10 -7 0.04 0.19 -8 10 -8 9.30 0.36 8 10 8 8.77 0.34 8 10 8 8.41 0.34 8 10 8 9.50 0.35 -8 10 -8 8.31 0.34 -8 -10 -8 8.45 0.33 -8 -10 -8 8.82 0.30 -8 10 -8 9.24 0.33 -8 -10 -8 8.10 0.35 -8 -10 -9 0.03 0.16 -8 10 -9 0.01 0.17 8 10 9 0.04 0.14 8 10 9 0.17 0.15 -8 10 -9 0.24 0.15 -8 -10 -9 0.13 0.14 -8 10 -9 0.06 0.15 -8 -10 -9 0.09 0.15 8 10 10 70.64 0.81 -8 -10 -10 65.85 0.72 -8 -10 -10 62.54 0.78 -8 10 -10 70.55 0.82 -8 -10 -10 63.36 0.81 -8 -10 -11 1.49 0.12 -8 10 -11 1.47 0.13 -8 12 9 7.97 0.20 -8 -12 9 8.85 0.19 -8 12 8 31.05 0.45 8 12 -8 31.68 0.46 8 12 -7 0.72 0.13 -8 -12 7 0.97 0.13 -8 12 7 0.54 0.14 -8 -12 7 0.60 0.13 -8 12 7 0.72 0.11 -8 -12 7 0.52 0.13 -8 -12 6 10.61 0.29 -8 12 6 11.37 0.27 -8 12 6 11.37 0.28 -8 -12 6 11.22 0.30 8 12 -6 11.03 0.32 -8 -12 6 11.01 0.33 8 12 -6 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1.10 0.45 -10 6 5 1.66 0.20 10 6 -5 1.56 0.47 -10 6 5 1.57 0.21 -10 -6 5 1.41 0.21 -10 6 5 1.34 0.22 10 6 -5 1.57 0.20 -10 -6 4 141.55 1.62 -10 -6 4 137.37 1.56 10 6 -4 139.76 1.62 10 -6 -4 137.12 2.75 10 6 -4 131.64 2.64 -10 -6 4 132.72 3.05 10 6 -4 135.56 1.53 -10 -6 4 140.10 1.65 -10 6 4 132.63 1.48 10 6 -4 129.14 2.88 -10 -6 4 138.57 1.64 -10 -6 3 3.59 0.29 -10 -6 3 3.20 0.27 10 6 -3 2.84 0.28 10 -6 -3 3.75 0.51 10 6 -3 3.89 0.56 -10 -6 3 4.47 0.54 -10 6 3 4.20 0.24 10 6 -3 3.33 0.25 -10 -6 3 3.33 0.30 10 6 -3 3.72 0.59 -10 -6 2 5.91 0.33 10 6 -2 5.92 0.34 10 6 -2 4.41 0.60 -10 -6 2 3.71 0.49 -10 6 2 3.52 0.22 10 6 -2 5.85 0.30 -10 -6 2 5.21 0.34 10 6 -2 4.46 0.62 10 6 -1 12.27 0.92 -10 -6 1 13.43 0.47 10 6 -1 12.75 0.45 -10 -6 1 13.17 0.47 -10 6 1 12.51 0.35 -10 -6 1 13.01 0.81 -10 -6 0 256.73 3.80 -10 6 0 236.10 4.06 10 6 0 241.83 4.19 -10 -6 0 245.79 2.48 -10 6 0 238.13 2.12 -10 -6 0 247.68 2.45 10 6 0 252.90 2.42 -10 -6 -1 19.65 0.56 10 6 1 19.78 0.54 -10 -6 -1 19.19 0.57 -10 6 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0.20 -10 -8 10 0.85 0.21 10 8 -10 0.73 0.23 -10 -8 10 0.68 0.19 -10 -8 9 0.01 0.22 -10 8 9 0.08 0.17 -10 8 9 -0.06 0.19 -10 -8 9 0.06 0.19 10 8 -9 0.03 0.23 -10 -8 9 0.10 0.19 -10 -8 9 -0.01 0.21 10 8 -9 0.16 0.19 -10 8 9 0.12 0.18 10 8 -9 -0.04 0.24 -10 8 9 0.02 0.18 -10 8 8 91.48 1.17 10 8 -8 89.63 1.25 -10 -8 8 90.00 1.24 -10 -8 8 86.98 1.20 -10 8 8 91.49 1.15 -10 -8 8 85.37 1.20 10 8 -8 88.98 1.28 -10 8 8 87.81 1.18 -10 8 7 0.89 0.21 -10 8 7 0.94 0.21 -10 -8 7 1.18 0.25 10 8 -7 1.23 0.25 -10 -8 7 0.99 0.24 -10 -8 7 0.87 0.23 -10 8 7 1.04 0.22 10 8 -7 1.17 0.29 -10 8 7 1.34 0.25 -10 8 6 406.62 3.51 -10 8 6 408.18 3.51 10 8 -6 406.91 3.62 -10 -8 6 407.96 3.61 -10 8 6 412.77 3.47 -10 -8 6 399.98 3.62 -10 8 6 411.81 3.58 -10 -8 5 5.05 0.37 -10 8 5 5.55 0.33 -10 8 5 5.12 0.31 -10 8 5 4.87 0.30 10 8 -5 5.10 0.34 -10 -8 5 5.44 0.35 -10 8 5 5.09 0.30 -10 8 5 5.40 0.34 -10 -8 5 5.58 0.36 10 8 -5 5.24 0.38 -10 -8 4 63.61 1.06 10 8 -4 63.56 1.08 10 8 -4 62.68 1.01 -10 -8 4 63.66 1.04 -10 -8 4 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3.91 0.26 -11 7 -7 24.75 0.65 11 7 7 26.86 0.71 11 7 7 24.51 0.63 -11 -7 -7 26.23 0.58 -11 7 -7 28.55 0.71 -11 -7 -7 25.56 0.53 -11 7 -7 24.68 0.57 11 7 7 26.15 0.55 -11 7 -7 25.19 0.64 -11 -7 -7 28.22 0.70 -11 -7 -8 6.42 0.37 -11 7 -8 6.84 0.38 11 7 8 6.19 0.39 11 7 8 7.11 0.36 -11 7 -8 6.91 0.39 -11 -7 -8 6.24 0.26 -11 7 -8 6.53 0.32 11 7 8 6.87 0.30 -11 7 -8 6.32 0.37 -11 -7 -8 6.07 0.30 11 7 9 107.22 1.39 11 7 9 111.59 1.31 -11 7 -9 110.52 1.36 -11 -7 -9 105.01 1.37 -11 -7 -9 104.00 1.23 -11 7 -9 108.89 1.29 11 7 9 112.39 1.21 -11 -7 -9 113.65 1.29 11 7 10 0.48 0.19 -11 7 -10 0.59 0.18 -11 -7 -10 0.53 0.18 11 7 10 0.49 0.15 -11 7 -10 0.55 0.19 11 7 10 0.59 0.16 11 7 11 15.28 0.40 -11 7 -11 16.15 0.40 11 7 11 16.21 0.35 -11 7 -11 16.76 0.40 11 7 12 0.40 0.11 11 7 12 0.53 0.15 -11 7 -12 0.49 0.13 -11 -7 -12 0.55 0.13 11 7 13 0.85 0.09 -11 -7 -13 0.74 0.11 -11 9 13 68.58 0.64 -11 -9 13 71.02 0.70 11 9 -12 19.33 0.35 -11 -9 12 20.56 0.39 -11 9 12 19.24 0.33 11 9 -12 18.38 0.43 -11 9 12 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0.35 -14 6 -1 10.55 0.38 -14 -6 -1 9.84 0.41 -14 -6 -2 149.42 1.86 -14 -6 -2 144.31 1.71 14 6 2 156.34 1.81 14 6 2 154.57 1.57 -14 6 -2 151.45 1.85 -14 6 -2 155.19 1.87 -14 6 -2 146.98 1.71 -14 -6 -2 146.65 1.53 -14 -6 -2 147.12 1.53 -14 6 -2 149.36 1.65 -14 6 -2 153.90 1.78 -14 6 -2 151.87 1.77 -14 6 -2 155.99 1.72 -14 6 -3 4.34 0.31 -14 6 -3 4.21 0.34 -14 -6 -3 4.43 0.37 14 6 3 3.73 0.24 14 6 3 4.08 0.32 -14 6 -3 4.68 0.37 -14 6 -3 4.87 0.40 -14 6 -3 4.31 0.34 -14 -6 -3 4.41 0.26 -14 6 -3 4.11 0.30 -14 -6 -3 4.65 0.32 -14 -6 -4 1.54 0.30 14 6 4 2.20 0.34 14 6 4 2.90 0.22 14 6 4 2.98 0.29 -14 -6 -4 2.45 0.24 -14 6 -4 1.27 0.28 -14 -6 -4 2.29 0.23 -14 6 -4 2.18 0.26 -14 -6 -4 1.22 0.24 14 6 5 17.36 0.42 14 6 5 17.00 0.52 -14 -6 -5 14.70 0.54 14 6 5 15.94 0.56 -14 -6 -5 15.45 0.43 -14 6 -5 17.16 0.54 -14 -6 -5 16.21 0.45 -14 6 -5 16.29 0.50 -14 -6 -5 14.98 0.49 14 6 6 82.86 1.00 14 6 6 84.93 1.15 14 6 6 85.01 1.26 -14 6 -6 85.55 1.22 -14 -6 -6 85.81 1.09 -14 -6 -6 82.16 1.15 14 6 7 1.34 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3.16 0.22 -14 -8 9 3.13 0.21 -14 8 9 3.03 0.22 -14 8 9 3.06 0.23 14 8 -9 3.28 0.26 14 8 -9 3.40 0.23 -14 -8 9 2.87 0.24 -14 -8 9 3.16 0.23 -14 -8 8 140.43 1.54 14 8 -8 139.50 1.58 -14 -8 8 149.38 1.47 -14 8 8 138.34 1.43 -14 8 8 141.48 1.46 14 8 -8 154.48 1.60 -14 8 8 147.88 1.49 14 8 -8 146.41 1.52 14 8 -8 138.97 1.48 -14 -8 8 143.35 1.58 -14 -8 7 6.18 0.33 14 8 -7 6.03 0.34 -14 -8 7 6.83 0.29 -14 8 7 6.53 0.30 -14 8 7 5.75 0.31 -14 8 7 6.51 0.31 -14 -8 7 6.18 0.31 14 8 -7 6.46 0.32 14 8 -7 5.94 0.29 -14 -8 7 5.84 0.32 14 8 -6 23.68 0.52 -14 -8 6 23.75 0.60 -14 -8 6 23.89 0.60 -14 8 6 23.73 0.55 -14 8 6 23.44 0.53 -14 8 6 25.27 0.56 -14 8 6 25.44 0.58 -14 8 6 24.30 0.55 -14 -8 6 23.24 0.53 14 8 -6 23.55 0.60 14 8 -6 23.81 0.55 -14 -8 5 5.07 0.33 -14 -8 5 4.43 0.31 -14 8 5 4.80 0.31 -14 8 5 4.38 0.27 -14 8 5 4.34 0.29 -14 8 5 4.78 0.32 -14 8 5 4.01 0.28 -14 -8 5 4.26 0.28 14 8 -5 4.34 0.31 14 8 -5 4.56 0.29 -14 -8 4 78.88 1.17 -14 -8 4 80.26 1.19 14 8 -4 77.41 1.15 -14 8 4 85.53 1.08 -14 8 4 77.77 1.10 -14 8 4 80.03 1.13 -14 8 4 82.62 1.09 -14 -8 4 79.36 1.05 14 8 -4 85.15 1.10 -14 8 4 84.68 1.15 -14 -8 3 0.10 0.21 -14 -8 3 -0.12 0.20 -14 8 3 0.36 0.23 -14 -8 3 0.24 0.24 14 8 -3 0.13 0.20 -14 8 3 0.32 0.19 -14 8 3 0.33 0.25 -14 8 3 0.12 0.20 -14 8 3 0.19 0.22 -14 -8 3 0.07 0.18 -14 8 3 0.18 0.22 14 8 -3 0.19 0.21 14 8 -3 0.12 0.20 -14 -8 2 33.86 0.76 -14 -8 2 31.30 0.66 -14 -8 2 33.51 0.76 14 8 -2 32.33 0.70 -14 8 2 34.82 0.65 -14 8 2 33.27 0.71 -14 8 2 33.00 0.69 -14 8 2 34.42 0.74 -14 8 2 34.20 0.68 -14 -8 2 32.74 0.62 14 8 -2 34.53 0.66 -14 8 2 35.03 0.73 14 8 -1 0.19 0.22 -14 -8 1 0.08 0.24 14 8 -1 0.16 0.17 -14 8 1 0.23 0.27 -14 8 1 0.35 0.24 -14 -8 1 0.06 0.17 -14 8 1 0.20 0.21 -14 -8 1 0.33 0.21 -14 8 1 0.00 0.17 14 8 -1 0.37 0.20 14 8 0 462.89 3.96 14 8 0 473.85 4.07 14 8 0 493.69 3.84 14 8 0 486.32 4.04 -14 8 0 476.13 4.07 -14 8 0 490.60 4.09 -14 8 0 476.18 3.94 -14 -8 0 475.68 3.78 -14 8 0 467.27 3.82 -14 -8 0 454.94 3.97 14 8 1 7.90 0.41 14 8 1 7.41 0.31 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3 3.89 0.24 -20 4 3 3.98 0.29 -20 4 2 26.95 0.57 -20 -4 2 27.87 0.60 -20 4 2 26.84 0.55 20 4 -2 27.79 0.52 -20 -4 2 27.27 0.54 -20 4 1 7.42 0.33 -20 4 1 6.65 0.29 -20 -4 1 7.22 0.31 -20 -4 1 6.70 0.25 -20 4 0 2.71 0.25 -20 -4 0 2.55 0.24 -20 4 0 2.45 0.20 -20 -4 0 2.11 0.22 -20 -4 0 2.52 0.19 -20 4 0 2.52 0.26 -20 -4 -1 5.13 0.25 -20 4 -1 5.12 0.29 -20 -4 -1 4.73 0.27 -20 -4 -2 73.70 0.93 -20 -4 -2 73.27 0.90 -20 -4 -2 76.29 0.92 -20 -4 -3 3.15 0.21 20 4 3 3.14 0.20 -20 -4 -3 3.56 0.21 -20 -4 -3 2.77 0.16 -20 -4 -3 3.32 0.21 -20 -4 -4 9.96 0.28 -20 -4 -4 10.02 0.30 -20 -4 -5 0.12 0.10 -20 -4 -5 0.26 0.13 -20 -4 -6 23.42 0.35 -20 -4 -7 0.08 0.07 -20 -4 -7 0.03 0.08 -20 6 9 0.69 0.09 -20 -6 9 1.03 0.09 -20 -6 8 0.21 0.09 -20 6 8 0.30 0.12 -20 6 7 0.56 0.14 -20 -6 7 0.41 0.10 -20 6 7 0.43 0.12 -20 6 6 79.16 0.91 -20 -6 6 81.92 0.86 -20 6 6 81.75 0.88 -20 6 5 3.99 0.18 -20 -6 5 4.40 0.22 -20 6 5 4.61 0.22 -20 6 5 4.34 0.25 20 6 -5 4.61 0.21 -20 -6 5 4.06 0.15 -20 -6 4 91.42 0.89 -20 -6 4 92.20 1.00 -20 -6 3 2.29 0.20 -20 6 3 2.43 0.19 20 6 -3 2.41 0.17 -20 -6 3 2.26 0.16 20 6 -2 1.67 0.16 -20 -6 2 1.63 0.16 -20 -6 1 1.21 0.17 20 6 -1 1.16 0.17 -20 -6 1 1.26 0.15 -20 -6 0 13.00 0.33 20 6 0 13.32 0.35 -20 -6 0 12.84 0.31 -20 -6 -1 8.93 0.26 20 6 1 8.47 0.28 -20 -6 -1 8.17 0.22 -20 -6 -1 8.88 0.26 -20 -6 -2 50.75 0.59 -20 -6 -3 0.23 0.10 -20 -6 -3 0.29 0.10 -20 -6 -4 0.52 0.10 -20 -6 -4 0.71 0.09 -20 -6 -5 0.58 0.07 -21 1 11 50.92 0.54 -21 -1 11 56.15 0.58 -21 1 10 5.70 0.20 -21 -1 10 5.57 0.21 -21 1 10 5.52 0.20 -21 -1 10 5.42 0.20 -21 1 9 0.49 0.14 -21 -1 9 0.64 0.15 -21 1 9 0.45 0.14 -21 -1 9 0.64 0.15 -21 1 9 0.60 0.11 -21 -1 9 0.44 0.11 -21 1 8 0.17 0.15 -21 1 8 0.07 0.15 -21 -1 8 0.18 0.16 -21 -1 8 0.11 0.12 -21 1 8 0.05 0.12 -21 -1 7 17.45 0.36 -21 -1 7 17.65 0.43 -21 -1 7 19.32 0.41 -21 1 7 19.02 0.41 -21 1 7 18.02 0.45 -21 -1 7 18.27 0.45 -21 -1 6 2.06 0.19 -21 1 6 1.99 0.18 -21 1 6 1.86 0.18 -21 -1 6 2.20 0.19 -21 1 6 2.12 0.22 -21 -1 6 2.01 0.21 -21 -1 6 2.07 0.20 -21 1 5 114.15 1.26 -21 -1 5 117.60 1.29 -21 1 5 116.29 1.32 -21 -1 5 117.53 1.31 -21 -1 5 122.11 1.28 -21 1 5 121.75 1.28 -21 1 5 116.90 1.34 -21 -1 5 115.56 1.34 -21 -1 5 119.28 1.30 -21 -1 4 1.16 0.21 -21 1 4 1.29 0.22 -21 1 4 1.28 0.22 -21 -1 4 0.96 0.21 -21 -1 4 1.41 0.19 -21 1 4 1.42 0.19 -21 1 4 1.37 0.23 -21 -1 4 1.29 0.23 -21 1 4 1.28 0.22 -21 -1 4 1.24 0.22 -21 1 3 231.23 2.15 -21 1 3 239.82 2.21 -21 -1 3 243.07 2.24 -21 -1 3 230.74 2.13 -21 -1 3 250.41 2.18 -21 1 3 245.80 2.17 -21 -1 3 244.32 2.20 -21 1 3 223.90 2.01 -21 1 3 232.93 2.18 -21 -1 3 238.39 2.21 -21 1 2 0.32 0.18 -21 1 2 0.26 0.17 -21 -1 2 0.28 0.18 -21 1 2 0.28 0.16 -21 -1 2 0.20 0.15 -21 1 2 0.07 0.20 -21 -1 2 0.12 0.20 -21 1 2 0.17 0.17 -21 1 1 4.35 0.26 -21 -1 1 3.91 0.25 -21 1 1 4.11 0.24 -21 -1 1 4.06 0.23 -21 1 1 4.03 0.28 -21 -1 1 4.00 0.28 -21 1 0 15.65 0.41 -21 -1 0 15.70 0.42 -21 -1 0 15.07 0.39 -21 1 0 14.61 0.40 -21 1 0 15.63 0.45 -21 -1 -1 0.81 0.17 -21 1 -1 0.72 0.16 -21 1 -1 0.69 0.17 -21 -1 -1 0.37 0.14 -21 1 -1 0.57 0.17 -21 -1 -1 0.49 0.17 -21 -1 -1 0.44 0.19 -21 -1 -2 0.59 0.15 -21 1 -2 0.69 0.17 -21 -1 -2 0.55 0.15 -21 1 -2 0.71 0.18 -21 -1 -2 0.60 0.17 -21 1 -2 0.59 0.19 -21 -1 -2 0.56 0.18 -21 1 -3 55.32 0.76 -21 -1 -3 54.81 0.75 -21 -1 -3 55.29 0.76 -21 -1 -3 53.21 0.69 -21 1 -3 54.41 0.76 -21 1 -3 53.85 0.73 -21 1 -4 1.32 0.16 -21 -1 -4 1.30 0.17 -21 -1 -4 1.12 0.15 -21 1 -4 1.40 0.18 -21 1 -4 1.23 0.17 -21 -1 -5 9.41 0.26 -21 -1 -5 9.33 0.28 -21 1 -5 9.46 0.28 -21 1 -6 0.19 0.11 -21 -1 -6 0.26 0.11 -21 1 -6 0.38 0.11 -21 -1 -7 0.75 0.09 -21 -1 -7 0.82 0.09 -21 3 10 0.07 0.11 -21 -3 10 0.16 0.09 -21 3 10 0.06 0.08 -21 -3 10 0.19 0.08 -21 3 9 18.28 0.36 -21 3 9 19.38 0.35 -21 -3 9 19.13 0.36 -21 3 8 0.02 0.14 -21 3 8 -0.03 0.13 -21 -3 8 0.06 0.13 -21 3 7 5.28 0.24 -21 -3 7 5.33 0.20 -21 -3 7 5.16 0.24 -21 -3 7 5.53 0.20 -21 3 7 5.31 0.20 -21 3 7 4.67 0.24 -21 -3 7 5.42 0.25 -21 -3 6 2.19 0.18 -21 -3 6 1.95 0.19 -21 -3 6 2.15 0.17 -21 -3 6 2.21 0.16 -21 3 6 2.10 0.16 -21 3 6 1.54 0.19 -21 3 6 2.19 0.20 -21 3 5 64.72 0.87 -21 3 5 64.79 0.79 -21 -3 5 67.70 0.86 -21 -3 5 65.34 0.84 -21 -3 5 67.31 0.83 -21 -3 5 68.90 0.79 -21 3 5 64.63 0.79 -21 3 5 63.50 0.86 -21 3 5 67.31 0.88 -21 -3 5 67.90 0.90 -21 -3 4 6.76 0.28 -21 3 4 6.49 0.29 -21 -3 4 6.29 0.30 -21 3 4 5.44 0.29 -21 3 4 6.00 0.28 -21 3 4 6.39 0.28 -21 -3 4 6.54 0.29 -21 -3 4 5.87 0.26 -21 -3 3 101.25 1.12 -21 3 3 97.46 1.11 -21 -3 3 97.56 1.14 -21 3 3 94.51 1.12 -21 3 3 98.52 1.13 -21 -3 3 100.05 1.17 -21 3 3 97.87 1.12 -21 -3 2 8.20 0.31 -21 -3 2 7.58 0.30 -21 3 2 7.92 0.31 -21 3 2 7.74 0.32 -21 -3 2 8.40 0.33 -21 3 2 7.23 0.29 -21 -3 1 4.70 0.25 -21 3 1 4.83 0.28 -21 3 1 4.73 0.23 -21 -3 1 4.31 0.20 -21 3 0 10.14 0.35 -21 -3 0 9.90 0.34 -21 -3 0 9.52 0.28 -21 -3 -1 7.58 0.30 -21 -3 -1 7.66 0.28 -21 -3 -1 7.89 0.27 21 3 1 7.62 0.27 -21 -3 -2 1.48 0.16 -21 3 -2 1.60 0.20 -21 -3 -2 1.37 0.18 -21 -3 -2 1.47 0.16 -21 -3 -3 48.99 0.64 -21 -3 -3 48.67 0.62 -21 -3 -4 0.05 0.10 -21 -3 -4 0.05 0.12 -21 -3 -5 14.42 0.30 -21 -3 -5 12.50 0.24 -21 -3 -6 0.04 0.06 -21 -5 8 0.24 0.09 -21 -5 8 0.19 0.08 -21 5 8 0.18 0.08 -21 -5 7 12.62 0.28 -21 -5 7 11.90 0.25 -21 5 7 12.20 0.27 -21 -5 6 0.49 0.11 -21 -5 6 0.47 0.11 -21 5 6 0.64 0.13 -21 5 5 73.03 0.86 -21 -5 5 72.48 0.73 -21 -5 4 0.19 0.14 -21 5 4 0.32 0.14 -21 5 4 0.26 0.16 -21 -5 4 0.18 0.12 -21 -5 3 132.15 1.28 -21 5 3 131.25 1.24 -21 -5 3 128.95 1.20 -21 -5 2 4.98 0.21 -21 5 2 4.59 0.21 21 5 -1 1.31 0.16 -21 -5 1 1.45 0.15 -21 -5 1 1.55 0.17 -21 -5 0 0.25 0.12 -21 -5 0 0.29 0.09 -21 -5 0 0.37 0.14 -21 -5 -1 5.12 0.17 -21 -5 -1 6.16 0.21 -21 -5 -2 0.89 0.11 -21 -5 -2 1.10 0.12 -21 -5 -3 71.67 0.71 -21 -5 -3 74.16 0.72 -21 -5 -4 0.11 0.07 -22 0 10 50.21 0.51 -22 0 9 -0.02 0.10 -22 0 9 0.09 0.10 -22 0 8 7.73 0.24 -22 0 7 0.05 0.10 -22 0 7 0.12 0.13 -22 0 6 6.87 0.27 -22 0 6 6.51 0.23 -22 0 6 6.36 0.21 -22 0 6 6.92 0.26 -22 0 5 -0.09 0.15 -22 0 5 -0.07 0.13 -22 0 5 -0.05 0.13 -22 0 5 0.15 0.13 -22 0 4 65.72 0.82 -22 0 4 67.62 0.84 -22 0 4 66.64 0.85 -22 0 4 67.97 0.86 -22 0 3 0.01 0.17 -22 0 3 0.04 0.16 -22 0 2 233.60 2.01 -22 0 2 233.99 1.97 -22 0 1 0.16 0.13 -22 0 1 0.04 0.17 -22 0 1 0.15 0.15 -22 0 0 10.50 0.29 -22 0 0 11.09 0.31 -22 0 -1 0.06 0.13 -22 0 -1 0.05 0.15 -22 0 -1 0.05 0.12 -22 0 -2 9.66 0.29 -22 0 -2 9.75 0.28 -22 0 -3 0.00 0.12 -22 0 -3 0.20 0.11 -22 0 -4 25.98 0.41 -22 2 9 0.20 0.09 -22 -2 9 0.27 0.09 -22 2 8 60.34 0.67 -22 -2 8 59.31 0.68 -22 -2 7 0.25 0.12 -22 -2 7 0.04 0.07 -22 -2 7 0.05 0.12 -22 2 6 21.97 0.42 -22 -2 6 22.45 0.37 -22 -2 6 21.66 0.41 -22 2 6 21.95 0.42 -22 2 5 3.68 0.21 -22 2 5 4.01 0.18 -22 -2 5 4.18 0.20 -22 -2 5 4.22 0.20 -22 2 5 4.20 0.21 -22 -2 5 4.29 0.22 -22 -2 5 4.38 0.21 -22 2 4 12.61 0.33 -22 2 4 13.23 0.33 -22 -2 4 13.31 0.34 -22 2 4 13.00 0.34 -22 -2 4 13.14 0.35 -22 -2 4 13.57 0.34 -22 2 3 3.97 0.22 -22 -2 3 4.03 0.24 -22 2 3 3.88 0.21 -22 2 3 3.56 0.20 -22 -2 3 3.69 0.21 -22 -2 3 4.01 0.22 -22 2 2 217.92 1.97 -22 -2 2 223.39 2.00 -22 2 1 12.03 0.35 -22 -2 1 11.93 0.35 -22 -2 1 11.24 0.26 -22 2 0 8.06 0.29 -22 -2 0 7.49 0.23 -22 -2 0 8.14 0.27 -22 -2 -1 14.18 0.34 -22 -2 -1 13.77 0.30 -22 -2 -1 14.74 0.33 -22 2 -2 4.89 0.22 -22 -2 -2 4.50 0.20 -22 -2 -2 4.63 0.19 -22 -2 -2 5.03 0.19 -22 -2 -3 0.52 0.12 -22 -2 -4 16.42 0.30 -22 -2 -5 3.62 0.13 -22 -4 7 0.38 0.07 -22 4 7 0.26 0.09 -22 -4 7 0.28 0.09 -22 4 7 0.14 0.09 -22 4 6 2.34 0.15 -22 -4 6 2.45 0.11 -22 -4 5 0.25 0.10 -22 4 5 0.24 0.10 -22 4 5 0.23 0.12 -22 -4 5 0.18 0.09 -22 -4 5 0.19 0.11 -22 4 4 19.54 0.36 -22 -4 4 19.46 0.36 -22 -4 4 19.65 0.33 -22 -4 3 1.31 0.15 -22 4 3 1.44 0.13 -22 -4 3 1.38 0.14 -22 -4 3 1.49 0.14 -22 -4 2 69.71 0.79 -22 -4 2 67.78 0.75 -22 -4 1 6.73 0.22 -22 -4 0 10.09 0.26 -22 -4 -1 1.36 0.12 -22 -4 -1 1.11 0.09 -22 -4 -1 1.37 0.12 -22 -4 -2 0.12 0.07 -22 -4 -2 0.20 0.08 -23 -1 7 40.98 0.46 -23 1 7 41.40 0.48 -23 -1 6 2.04 0.11 -23 1 6 2.15 0.12 -23 1 6 2.14 0.13 -23 -1 6 2.25 0.13 -23 1 5 0.63 0.08 -23 -1 5 0.63 0.10 -23 1 5 0.68 0.10 -23 1 5 0.77 0.11 -23 -1 5 0.74 0.11 -23 1 4 0.05 0.09 -23 -1 4 0.05 0.10 -23 1 4 0.02 0.09 -23 -1 4 -0.08 0.10 -23 1 3 15.17 0.31 -23 -1 3 16.09 0.32 -23 1 2 5.07 0.20 -23 -1 2 5.34 0.21 -23 1 1 149.79 1.34 -23 -1 1 149.01 1.34 -23 -1 0 0.20 0.08 -23 1 0 0.27 0.13 -23 -1 0 0.21 0.10 -23 1 -1 16.83 0.31 -23 -1 -1 16.60 0.31 -23 -1 -2 -0.01 0.07 -23 -1 -2 0.03 0.07 -23 3 6 0.34 0.07 -23 -3 6 0.34 0.07 -23 3 5 14.17 0.24 -23 -3 5 14.06 0.24 -23 3 4 2.60 0.11 -23 -3 4 2.35 0.11 -23 -3 3 0.17 0.09 -23 -3 3 0.21 0.09 -23 -3 2 1.37 0.12 -23 -3 2 1.57 0.12 -23 -3 0 2.51 0.13 -23 -3 0 3.02 0.13 TITL 3Pic1A_auto in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 18.799044 11.303307 15.863936 90.0000 96.8250 90.0000 ZERR 5.00 0.000110 0.000055 0.000080 0.0000 0.0005 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N S Ni UNIT 140.00 155.00 35.00 10.00 5.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6217 _shelx_res_file ; TITL 3pic1_auto_a.res in C2/c 3pic1a.res created by SHELXL-2016/6 at 14:45:45 on 12-May-2022 REM Old TITL 3Pic1_auto in C2/c REM SHELXT solution in C2/c REM R1 0.152, Rweak 0.008, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C22 N10 S2 Ni CELL 1.54184 18.799 11.3033 15.8639 90 96.825 90 ZERR 4 0.0001 0.0001 0.0001 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Ni S UNIT 120 136 32 4 8 EQIV $1 1-X,+Y,1.5-Z EQIV $2 0.5-X,0.5+Y,1.5-Z RIGU C22 C23 C24 C25 C26 RIGU C22' C23' C24' C25' C26' DFIX 1.1 N31 C31 DFIX 1.45 C31 C32 RIGU 0.0001 0.0001 N31 C31 C32 DFIX 1.1 N31' C31' DFIX 1.45 C31' C32' RIGU 0.0001 0.0001 N31' C31' C32' L.S. 10 PLAN 5 SIZE 0.05 0.15 0.25 TEMP -173.14(10) HTAB C25' N21_$1 HTAB C32 S1_$2 HTAB C32' S1 BOND $H HTAB fmap 2 ACTA OMIT 0 2 4 OMIT 2 0 2 REM REM REM WGHT 0.096500 2.692000 FVAR 0.28637 0.75671 NI1 4 0.500000 0.248898 0.750000 10.50000 0.02657 0.02410 = 0.02722 0.00000 0.00339 0.00000 N1 3 0.420207 0.248921 0.827814 11.00000 0.03280 0.03472 = 0.03671 0.00120 0.00759 -0.00036 C1 1 0.365113 0.247940 0.853459 11.00000 0.03358 0.02572 = 0.02536 0.00063 0.00093 0.00156 S1 5 0.287269 0.246112 0.889846 11.00000 0.02965 0.04879 = 0.04307 0.00200 0.00930 0.00236 N11 3 0.556649 0.380534 0.826373 11.00000 0.03605 0.02857 = 0.03457 -0.00368 0.00441 -0.00346 C11 1 0.522593 0.471538 0.857503 11.00000 0.04524 0.03237 = 0.03949 -0.00573 0.00995 -0.00264 AFIX 43 H11 2 0.472097 0.476613 0.843833 11.00000 -1.20000 AFIX 0 C12 1 0.556966 0.559424 0.908890 11.00000 0.06494 0.03908 = 0.04914 -0.01370 0.01663 -0.00992 C13 1 0.630256 0.549681 0.929370 11.00000 0.06090 0.06014 = 0.06113 -0.02587 0.00667 -0.02232 AFIX 43 H13 2 0.655637 0.607165 0.964830 11.00000 -1.20000 AFIX 0 C14 1 0.666402 0.456448 0.898250 11.00000 0.04247 0.06600 = 0.07287 -0.02111 -0.00228 -0.01324 AFIX 43 H14 2 0.716769 0.448707 0.911946 11.00000 -1.20000 AFIX 0 C15 1 0.627942 0.374154 0.846599 11.00000 0.03645 0.04306 = 0.05385 -0.01115 0.00012 -0.00423 AFIX 43 H15 2 0.653079 0.310505 0.824553 11.00000 -1.20000 AFIX 0 C16 1 0.515142 0.661315 0.938822 11.00000 0.08890 0.05805 = 0.08497 -0.03318 0.02691 -0.00642 AFIX 137 H16A 2 0.509929 0.722969 0.895090 11.00000 -1.50000 H16B 2 0.540591 0.693673 0.991274 11.00000 -1.50000 H16C 2 0.467636 0.633742 0.949620 11.00000 -1.50000 AFIX 0 SAME 0.02 0.04 N11 C11 C12 C13 C14 C15 C16 N21 3 0.444322 0.115385 0.674645 11.00000 0.03525 0.02951 = 0.02762 0.00094 0.00081 -0.00482 C21 1 0.437638 0.120221 0.589792 11.00000 0.03935 0.03299 = 0.02880 0.00183 0.00384 -0.00213 PART 1 AFIX 43 H21 2 0.460555 0.183760 0.564569 21.00000 -1.20000 AFIX 43 PART 2 H21A 2 0.452665 0.188327 0.561597 -21.00000 -1.20000 AFIX 0 PART 1 C22 1 0.400486 0.041013 0.536773 21.00000 0.04086 0.03128 = 0.03245 0.00121 0.00581 -0.00109 C23 1 0.368344 -0.053515 0.574077 21.00000 0.04559 0.03676 = 0.03688 -0.00516 0.00114 -0.01382 AFIX 43 H23 2 0.343460 -0.112681 0.539724 21.00000 -1.20000 AFIX 0 C24 1 0.373025 -0.060332 0.661474 21.00000 0.05352 0.04088 = 0.04109 0.00193 0.00441 -0.01965 AFIX 43 H24 2 0.350897 -0.123617 0.687939 21.00000 -1.20000 AFIX 0 C25 1 0.410003 0.025387 0.709497 21.00000 0.04061 0.04117 = 0.03147 0.00531 0.00065 -0.01402 AFIX 43 H25 2 0.411687 0.021686 0.769528 21.00000 -1.20000 AFIX 0 C26 1 0.398119 0.053254 0.441966 21.00000 0.06160 0.04820 = 0.02942 -0.00576 0.00321 -0.01220 AFIX 137 H26A 2 0.368378 0.121456 0.422608 21.00000 -1.50000 H26B 2 0.377644 -0.018657 0.414374 21.00000 -1.50000 H26C 2 0.446794 0.064930 0.427212 21.00000 -1.50000 AFIX 0 PART 2 C22' 1 0.406197 0.016841 0.540331 -21.00000 0.06448 0.03720 = 0.01881 -0.01178 -0.01981 0.01445 AFIX 43 H22' 2 0.398402 0.020171 0.480103 -21.00000 -1.20000 AFIX 0 C23' 1 0.388959 -0.080953 0.581299 -21.00000 0.05299 0.04172 = 0.04478 -0.00903 -0.01219 -0.00017 AFIX 43 H23' 2 0.367339 -0.146067 0.550209 -21.00000 -1.20000 AFIX 0 C24' 1 0.402459 -0.086901 0.667507 -21.00000 0.03441 0.03592 = 0.03802 -0.00399 -0.00408 -0.00424 C25' 1 0.432233 0.014696 0.711500 -21.00000 0.02117 0.02978 = 0.02864 -0.00199 -0.00833 -0.00622 AFIX 43 H25' 2 0.444086 0.009232 0.771277 -21.00000 -1.20000 AFIX 0 C26' 1 0.390974 -0.197789 0.717906 -21.00000 0.06293 0.04463 = 0.04987 0.00148 -0.01029 -0.02459 AFIX 137 H26D 2 0.349846 -0.241696 0.689851 -21.00000 -1.50000 H26E 2 0.381743 -0.175834 0.775373 -21.00000 -1.50000 H26F 2 0.433910 -0.247524 0.721077 -21.00000 -1.50000 AFIX 0 PART 1 N31 3 0.395484 0.691749 0.791082 10.50000 0.18844 0.15307 = 0.14606 0.06657 0.00283 0.00663 C31 1 0.345370 0.647467 0.806851 10.50000 0.17756 0.09831 = 0.09629 0.03978 -0.00177 0.02469 C32 1 0.277526 0.591873 0.817288 10.50000 0.17198 0.09907 = 0.20224 0.09179 0.00033 0.03752 AFIX 137 H32A 2 0.241992 0.613118 0.769401 10.50000 -1.50000 H32B 2 0.261097 0.619130 0.870340 10.50000 -1.50000 H32C 2 0.283598 0.505767 0.819183 10.50000 -1.50000 AFIX 0 PART 2 N31' 3 0.278809 0.711648 0.919833 10.50000 0.12839 0.13142 = 0.22066 0.03108 -0.01565 0.04943 C31' 1 0.285364 0.643132 0.867675 10.50000 0.05125 0.08707 = 0.19684 0.06152 -0.00054 0.01092 C32' 1 0.293739 0.558773 0.806678 10.50000 0.10046 0.07661 = 0.18353 0.07567 0.00036 0.02499 AFIX 137 H32D 2 0.328828 0.586604 0.770166 10.50000 -1.50000 H32E 2 0.247670 0.545062 0.772217 10.50000 -1.50000 H32F 2 0.310663 0.484778 0.834360 10.50000 -1.50000 AFIX 0 HKLF 4 REM 3pic1_auto_a.res in C2/c REM R1 = 0.0456 for 3462 Fo > 4sig(Fo) and 0.0463 for all 3605 data REM 264 parameters refined using 82 restraints END WGHT 0.0965 2.6920 REM Instructions for potential hydrogen bonds HTAB C25' N21_$1 HTAB C32 S1_$2 HTAB C32' S1 REM Highest difference peak 0.799, deepest hole -0.461, 1-sigma level 0.064 Q1 1 0.3196 0.7167 0.8493 11.00000 0.05 0.80 Q2 1 0.3378 0.1981 0.3588 11.00000 0.05 0.77 Q3 1 0.7410 0.4199 0.9284 11.00000 0.05 0.57 Q4 1 0.6367 0.4714 0.9286 11.00000 0.05 0.34 Q5 1 0.5907 0.5405 0.9445 11.00000 0.05 0.34 ; _shelx_res_checksum 26430 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni1 0.500000 0.24890(3) 0.750000 0.02595(17) Uani d 1 A . N N1 0.42021(9) 0.24892(10) 0.82781(11) 0.0345(4) Uani d 1 . . C C1 0.36511(10) 0.24794(11) 0.85346(11) 0.0284(4) Uani d 1 . . S S1 0.28727(2) 0.24611(4) 0.88985(3) 0.04010(18) Uani d 1 . . N N11 0.55665(7) 0.38053(12) 0.82637(9) 0.0330(3) Uani d 1 . . C C11 0.52259(10) 0.47154(15) 0.85750(11) 0.0386(4) Uani d 1 . . H H11 0.472097 0.476613 0.843833 0.046 Uiso calc 1 . . C C12 0.55697(12) 0.55942(17) 0.90889(13) 0.0503(5) Uani d 1 . . C C13 0.63026(13) 0.5497(2) 0.92937(16) 0.0608(6) Uani d 1 . . H H13 0.655637 0.607165 0.964830 0.073 Uiso calc 1 . . C C14 0.66640(11) 0.4564(2) 0.89825(16) 0.0612(6) Uani d 1 . . H H14 0.716769 0.448707 0.911946 0.073 Uiso calc 1 . . C C15 0.62794(9) 0.37415(17) 0.84660(12) 0.0449(4) Uani d 1 . . H H15 0.653079 0.310505 0.824553 0.054 Uiso calc 1 . . C C16 0.51514(16) 0.6613(2) 0.93882(19) 0.0760(8) Uani d 1 . . H H16A 0.509929 0.722969 0.895090 0.114 Uiso calc 1 . . H H16B 0.540591 0.693673 0.991274 0.114 Uiso calc 1 . . H H16C 0.467636 0.633742 0.949620 0.114 Uiso calc 1 . . N N21 0.44432(7) 0.11538(12) 0.67464(8) 0.0310(3) Uani d 1 . . C C21 0.43764(9) 0.12022(14) 0.58979(10) 0.0337(3) Uani d 1 . . H H21 0.460555 0.183760 0.564569 0.040 Uiso calc 0.757(5) A 1 H H21A 0.452665 0.188327 0.561597 0.040 Uiso calc 0.243(5) A 2 C C22 0.4005(3) 0.0410(5) 0.5368(4) 0.0347(12) Uani d 0.757(5) A 1 C C23 0.3683(3) -0.0535(4) 0.5741(3) 0.0400(9) Uani d 0.757(5) A 1 H H23 0.343460 -0.112681 0.539724 0.048 Uiso calc 0.757(5) A 1 C C24 0.3730(2) -0.0603(3) 0.6615(2) 0.0453(8) Uani d 0.757(5) A 1 H H24 0.350897 -0.123617 0.687939 0.054 Uiso calc 0.757(5) A 1 C C25 0.4100(2) 0.0254(5) 0.7095(4) 0.0380(11) Uani d 0.757(5) A 1 H H25 0.411687 0.021686 0.769528 0.046 Uiso calc 0.757(5) A 1 C C26 0.39812(15) 0.0533(2) 0.44197(14) 0.0466(7) Uani d 0.757(5) A 1 H H26A 0.368378 0.121456 0.422608 0.070 Uiso calc 0.757(5) A 1 H H26B 0.377644 -0.018657 0.414374 0.070 Uiso calc 0.757(5) A 1 H H26C 0.446794 0.064930 0.427212 0.070 Uiso calc 0.757(5) A 1 C C22' 0.4062(13) 0.017(2) 0.5403(11) 0.042(4) Uani d 0.243(5) A 2 H H22' 0.398402 0.020171 0.480103 0.051 Uiso calc 0.243(5) A 2 C C23' 0.3890(8) -0.0810(15) 0.5813(11) 0.048(3) Uani d 0.243(5) A 2 H H23' 0.367339 -0.146067 0.550209 0.058 Uiso calc 0.243(5) A 2 C C24' 0.4025(5) -0.0869(9) 0.6675(6) 0.0368(19) Uani d 0.243(5) A 2 C C25' 0.4322(6) 0.0147(15) 0.7115(12) 0.027(2) Uani d 0.243(5) A 2 H H25' 0.444086 0.009232 0.771277 0.033 Uiso calc 0.243(5) A 2 C C26' 0.3910(5) -0.1978(8) 0.7179(5) 0.054(2) Uani d 0.243(5) A 2 H H26D 0.349846 -0.241696 0.689851 0.081 Uiso calc 0.243(5) A 2 H H26E 0.381743 -0.175834 0.775373 0.081 Uiso calc 0.243(5) A 2 H H26F 0.433910 -0.247524 0.721077 0.081 Uiso calc 0.243(5) A 2 N N31 0.3955(6) 0.6917(11) 0.7911(7) 0.164(3) Uani d 0.5 B 1 C C31 0.3454(6) 0.6475(8) 0.8069(6) 0.126(2) Uani d 0.5 B 1 C C32 0.2775(8) 0.5919(12) 0.8173(13) 0.160(5) Uani d 0.5 B 1 H H32A 0.241992 0.613118 0.769401 0.239 Uiso calc 0.5 B 1 H H32B 0.261097 0.619130 0.870340 0.239 Uiso calc 0.5 B 1 H H32C 0.283598 0.505767 0.819183 0.239 Uiso calc 0.5 B 1 N N31' 0.2788(5) 0.7116(10) 0.9198(8) 0.163(3) Uani d 0.5 C 2 C C31' 0.2854(4) 0.6431(8) 0.8677(8) 0.113(2) Uani d 0.5 C 2 C C32' 0.2937(5) 0.5588(9) 0.8067(11) 0.122(3) Uani d 0.5 C 2 H H32D 0.328828 0.586604 0.770166 0.182 Uiso calc 0.5 C 2 H H32E 0.247670 0.545062 0.772217 0.182 Uiso calc 0.5 C 2 H H32F 0.310663 0.484778 0.834360 0.182 Uiso calc 0.5 C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0266(3) 0.0241(3) 0.0272(3) 0.000 0.00339(17) 0.000 N1 0.0328(8) 0.0347(8) 0.0367(8) -0.0004(4) 0.0076(6) 0.0012(5) C1 0.0336(8) 0.0257(8) 0.0254(8) 0.0016(5) 0.0009(6) 0.0006(4) S1 0.0297(3) 0.0488(3) 0.0431(3) 0.00236(14) 0.0093(2) 0.00200(15) N11 0.0360(7) 0.0286(6) 0.0346(7) -0.0035(5) 0.0044(5) -0.0037(5) C11 0.0452(9) 0.0324(8) 0.0395(8) -0.0026(7) 0.0099(7) -0.0057(6) C12 0.0649(12) 0.0391(9) 0.0491(10) -0.0099(8) 0.0166(9) -0.0137(8) C13 0.0609(13) 0.0601(13) 0.0611(13) -0.0223(11) 0.0067(10) -0.0259(11) C14 0.0425(10) 0.0660(14) 0.0729(14) -0.0132(9) -0.0023(9) -0.0211(11) C15 0.0364(8) 0.0431(9) 0.0538(10) -0.0042(7) 0.0001(7) -0.0112(8) C16 0.0889(19) 0.0580(14) 0.0850(18) -0.0064(12) 0.0269(15) -0.0332(13) N21 0.0352(7) 0.0295(6) 0.0276(6) -0.0048(5) 0.0008(5) 0.0009(5) C21 0.0393(8) 0.0330(8) 0.0288(7) -0.0021(6) 0.0038(6) 0.0018(6) C22 0.0409(18) 0.031(2) 0.0324(18) -0.0011(17) 0.0058(14) 0.0012(12) C23 0.046(2) 0.037(2) 0.0369(16) -0.0138(16) 0.0011(16) -0.0052(13) C24 0.054(2) 0.0409(17) 0.0411(14) -0.0197(15) 0.0044(15) 0.0019(12) C25 0.041(3) 0.0412(18) 0.0315(15) -0.014(2) 0.001(2) 0.0053(12) C26 0.0616(15) 0.0482(14) 0.0294(11) -0.0122(11) 0.0032(10) -0.0058(9) C22' 0.064(8) 0.037(7) 0.019(4) 0.014(5) -0.020(4) -0.012(4) C23' 0.053(8) 0.042(6) 0.045(4) 0.000(5) -0.012(5) -0.009(4) C24' 0.034(5) 0.036(4) 0.038(3) -0.004(3) -0.004(3) -0.004(3) C25' 0.021(6) 0.030(4) 0.029(4) -0.006(4) -0.008(4) -0.002(3) C26' 0.063(5) 0.045(4) 0.050(4) -0.025(4) -0.010(4) 0.001(3) N31 0.188(4) 0.153(7) 0.146(7) 0.007(4) 0.003(4) 0.067(6) C31 0.178(4) 0.098(5) 0.096(5) 0.025(3) -0.002(4) 0.040(4) C32 0.172(5) 0.099(9) 0.202(14) 0.038(4) 0.000(5) 0.092(9) N31' 0.128(7) 0.131(5) 0.221(5) 0.049(5) -0.016(4) 0.031(4) C31' 0.051(3) 0.087(4) 0.197(5) 0.011(3) -0.001(4) 0.062(3) C32' 0.100(5) 0.077(4) 0.184(5) 0.025(4) 0.000(4) 0.076(3) 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' S S 0.3331 0.5567 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ni1 N1 2_656 . 179.99(7) ? N1 Ni1 N11 2_656 2_656 90.55(6) ? N1 Ni1 N11 . 2_656 89.44(6) ? N1 Ni1 N11 . . 90.55(6) ? N1 Ni1 N11 2_656 . 89.44(6) ? N1 Ni1 N21 2_656 . 90.46(6) ? N1 Ni1 N21 . . 89.55(6) ? N1 Ni1 N21 . 2_656 90.46(6) ? N1 Ni1 N21 2_656 2_656 89.55(6) ? N11 Ni1 N11 . 2_656 91.03(8) ? N21 Ni1 N11 2_656 . 89.80(6) ? N21 Ni1 N11 2_656 2_656 179.16(5) ? N21 Ni1 N11 . 2_656 89.80(6) ? N21 Ni1 N11 . . 179.16(5) ? N21 Ni1 N21 . 2_656 89.36(7) ? C1 N1 Ni1 . . 163.77(15) ? N1 C1 S1 . . 179.81(16) ? C11 N11 Ni1 . . 121.35(11) ? C11 N11 C15 . . 117.48(15) ? C15 N11 Ni1 . . 121.16(11) ? N11 C11 H11 . . 118.1 ? N11 C11 C12 . . 123.73(17) ? C12 C11 H11 . . 118.1 ? C11 C12 C16 . . 120.5(2) ? C13 C12 C11 . . 117.42(18) ? C13 C12 C16 . . 122.1(2) ? C12 C13 H13 . . 120.1 ? C14 C13 C12 . . 119.83(19) ? C14 C13 H13 . . 120.1 ? C13 C14 H14 . . 120.6 ? C13 C14 C15 . . 118.7(2) ? C15 C14 H14 . . 120.6 ? N11 C15 C14 . . 122.78(18) ? N11 C15 H15 . . 118.6 ? C14 C15 H15 . . 118.6 ? C12 C16 H16A . . 109.5 ? C12 C16 H16B . . 109.5 ? C12 C16 H16C . . 109.5 ? H16A C16 H16B . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? C21 N21 Ni1 . . 121.24(10) ? C21 N21 C25 . . 116.6(3) ? C25 N21 Ni1 . . 122.0(3) ? C25' N21 Ni1 . . 117.8(8) ? C25' N21 C21 . . 118.9(8) ? N21 C21 H21 . . 117.5 ? N21 C21 H21A . . 120.6 ? N21 C21 C22 . . 125.0(2) ? N21 C21 C22' . . 118.8(8) ? C22 C21 H21 . . 117.5 ? C22' C21 H21A . . 120.6 ? C21 C22 C23 . . 117.3(4) ? C21 C22 C26 . . 120.5(3) ? C23 C22 C26 . . 122.1(5) ? C22 C23 H23 . . 120.3 ? C24 C23 C22 . . 119.3(4) ? C24 C23 H23 . . 120.3 ? C23 C24 H24 . . 120.4 ? C25 C24 C23 . . 119.1(4) ? C25 C24 H24 . . 120.4 ? N21 C25 C24 . . 122.5(5) ? N21 C25 H25 . . 118.7 ? C24 C25 H25 . . 118.7 ? C22 C26 H26A . . 109.5 ? C22 C26 H26B . . 109.5 ? C22 C26 H26C . . 109.5 ? H26A C26 H26B . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? C21 C22' H22' . . 120.2 ? C23' C22' C21 . . 119.6(14) ? C23' C22' H22' . . 120.2 ? C22' C23' H23' . . 120.0 ? C22' C23' C24' . . 120.0(15) ? C24' C23' H23' . . 120.0 ? C23' C24' C25' . . 117.9(13) ? C23' C24' C26' . . 123.3(10) ? C25' C24' C26' . . 118.7(11) ? N21 C25' C24' . . 124.1(15) ? N21 C25' H25' . . 118.0 ? C24' C25' H25' . . 118.0 ? C24' C26' H26D . . 109.5 ? C24' C26' H26E . . 109.5 ? C24' C26' H26F . . 109.5 ? H26D C26' H26E . . 109.5 ? H26D C26' H26F . . 109.5 ? H26E C26' H26F . . 109.5 ? N31 C31 C32 . . 173.6(12) ? C31 C32 H32A . . 109.5 ? C31 C32 H32B . . 109.5 ? C31 C32 H32C . . 109.5 ? H32A C32 H32B . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? N31' C31' C32' . . 178.5(12) ? C31' C32' H32D . . 109.5 ? C31' C32' H32E . . 109.5 ? C31' C32' H32F . . 109.5 ? H32D C32' H32E . . 109.5 ? H32D C32' H32F . . 109.5 ? H32E C32' H32F . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 N1 2_656 2.0528(16) ? Ni1 N1 . 2.0528(16) y Ni1 N11 . 2.1235(14) y Ni1 N11 2_656 2.1235(13) ? Ni1 N21 . 2.1224(13) y Ni1 N21 2_656 2.1224(13) ? N1 C1 . 1.157(3) ? C1 S1 . 1.6358(19) ? N11 C11 . 1.337(2) ? N11 C15 . 1.342(2) ? C11 H11 . 0.9500 ? C11 C12 . 1.394(2) ? C12 C13 . 1.382(3) ? C12 C16 . 1.503(3) ? C13 H13 . 0.9500 ? C13 C14 . 1.377(3) ? C14 H14 . 0.9500 ? C14 C15 . 1.385(3) ? C15 H15 . 0.9500 ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C16 H16C . 0.9800 ? N21 C21 . 1.3381(19) ? N21 C25 . 1.357(6) ? N21 C25' . 1.312(19) ? C21 H21 . 0.9500 ? C21 H21A . 0.9500 ? C21 C22 . 1.363(6) ? C21 C22' . 1.490(19) ? C22 C23 . 1.394(6) ? C22 C26 . 1.506(6) ? C23 H23 . 0.9500 ? C23 C24 . 1.381(5) ? C24 H24 . 0.9500 ? C24 C25 . 1.370(7) ? C25 H25 . 0.9500 ? C26 H26A . 0.9800 ? C26 H26B . 0.9800 ? C26 H26C . 0.9800 ? C22' H22' . 0.9500 ? C22' C23' . 1.34(2) ? C23' H23' . 0.9500 ? C23' C24' . 1.363(19) ? C24' C25' . 1.423(19) ? C24' C26' . 1.516(13) ? C25' H25' . 0.9500 ? C26' H26D . 0.9800 ? C26' H26E . 0.9800 ? C26' H26F . 0.9800 ? N31 C31 . 1.121(11) ? C31 C32 . 1.449(14) ? C32 H32A . 0.9800 ? C32 H32B . 0.9800 ? C32 H32C . 0.9800 ? N31' C31' . 1.151(12) ? C31' C32' . 1.381(15) ? C32' H32D . 0.9800 ? C32' H32E . 0.9800 ? C32' H32F . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C25' H25' N21 2_656 0.95 2.48 2.991(15) 113.7 C32 H32A S1 4_556 0.98 2.93 3.791(17) 146.5 C32' H32F S1 . 0.98 2.89 3.779(10) 151.7 _cod_database_fobs_code 2244208