#------------------------------------------------------------------------------ #$Date: 2023-06-29 17:51:03 +0200 (Thu, 29 Jun 2023) $ #$Revision: 284695 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022796.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_2022796 loop_ _publ_author_name 'Golen, James A.' 'Manke, David R.' _publ_section_title ; 3,5-Lutidine pentaaqua sulfate complexes of first-row transition metals: [M(3,5-lutidine)(H2O)5]SO4, with M = Mn, Co, Ni, and Zn ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989023005261 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac '[Ni (C7 H9 N) (H2 O)5] S O4' _chemical_formula_moiety 'C7 H19 Ni N O5 2+, O4 S 2-' _chemical_formula_sum 'C7 H19 N Ni O9 S' _chemical_formula_weight 352.00 _chemical_name_systematic ; Pentaaqua(3,5-dimethylpyridine-\kN)nickel(II) sulfate ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.1196(8) _cell_length_b 7.0609(3) _cell_length_c 11.2233(5) _cell_measurement_reflns_used 9899 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 26.31 _cell_measurement_theta_min 2.99 _cell_volume 1356.67(10) _computing_cell_refinement ; SAINT (Bruker, 2021) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2021) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 297.15 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 Venture CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_unetI/netI 0.0127 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 36924 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.392 _diffrn_reflns_theta_min 3.611 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2021) ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.723 _exptl_crystal_description BLOCK _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.436 _refine_diff_density_min -0.334 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 1499 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0228 _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^)+(0.0308P)^2^+0.6821P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.0595 _reflns_number_gt 1386 _reflns_number_total 1499 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zv2026sup1.cif _cod_data_source_block 3 _cod_database_code 2022796 _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 0.770 _shelx_estimated_absorpt_t_max 0.953 _shelx_hkl_file ; 0 -1 0 5.20 2.10 0 -1 0 -1.80 1.70 0 1 0 5.50 2.30 0 1 0 -0.50 1.50 0 -1 0 6.90 1.40 0 1 0 1.20 1.30 0 -3 0 1.30 4.20 0 3 0 1.20 4.20 0 3 0 0.00 2.80 0 3 0 2.40 3.50 0 3 0 0.80 2.60 0 -3 0 3.50 2.70 0 4 0 9762.22 177.88 0 4 0 9816.32 176.38 0 -4 0 9999.00 178.28 0 -5 0 6.10 5.80 0 -5 0 -0.80 5.00 0 -5 0 -3.00 2.90 0 5 0 4.40 5.60 0 -5 0 -2.00 3.30 0 5 0 1.90 3.60 0 5 0 1.40 4.10 0 5 0 -3.70 3.20 0 -6 0 3303.07 65.69 0 -6 0 3350.86 70.29 0 -6 0 3325.27 72.59 0 -6 0 3297.07 64.19 0 6 0 3382.26 65.79 0 6 0 3342.67 65.29 0 6 0 3281.37 74.39 0 -7 0 12.40 7.60 0 -7 0 -3.80 6.70 0 -7 0 -4.50 4.00 0 7 0 -0.30 6.80 0 7 0 2.10 4.70 0 -7 0 -1.80 3.90 0 7 0 -3.70 4.00 0 8 0 649.83 26.40 0 8 0 671.33 29.50 0 -8 0 684.93 29.00 0 8 0 637.24 20.10 0 -8 0 656.93 21.80 0 -8 0 629.94 19.60 0 -2 1 0.10 1.80 0 2 -1 1.50 3.00 0 2 -1 0.00 2.70 0 -2 -1 3.00 3.50 0 2 1 2.60 3.20 0 -2 1 0.20 1.80 0 -2 1 1.20 2.60 0 2 1 -3.00 3.20 0 2 -1 0.30 3.80 0 -2 1 2.60 3.70 0 -2 -1 -2.90 2.20 0 -2 -1 -0.50 3.30 0 2 -1 -0.80 1.80 0 -2 -1 -4.40 3.00 0 3 1 54.19 4.80 0 -3 -1 51.29 6.20 0 -3 1 49.99 4.00 0 3 1 46.40 5.80 0 3 -1 51.09 4.20 0 -3 1 49.30 5.00 0 3 -1 37.40 5.70 0 -3 -1 45.60 5.70 0 3 -1 56.39 5.60 0 -3 1 43.50 5.80 0 -3 -1 53.39 6.10 0 -3 -1 58.19 4.90 0 3 1 48.50 5.50 0 3 -1 61.69 6.20 0 4 1 8.00 5.10 0 -4 -1 1.00 2.80 0 4 1 -1.80 3.10 0 4 -1 0.50 3.20 0 -4 1 2.60 4.50 0 4 -1 0.50 2.60 0 -4 1 1.60 2.60 0 4 -1 -0.30 4.00 0 4 1 -0.60 4.10 0 -4 -1 2.80 4.30 0 -4 1 -2.10 3.20 0 4 -1 -2.50 4.50 0 -4 -1 -2.70 4.20 0 -5 1 1686.93 35.00 0 5 1 1778.12 40.60 0 -5 -1 1711.53 36.50 0 5 -1 1725.03 42.60 0 5 1 1700.53 42.00 0 5 1 1750.62 38.30 0 5 -1 1748.03 37.60 0 5 -1 1809.62 40.70 0 -5 1 1749.03 40.20 0 -5 1 1775.52 42.70 0 -5 -1 1712.23 41.00 0 -5 1 1711.03 37.50 0 -5 -1 1722.03 41.90 0 5 -1 1753.42 35.70 0 -6 -1 -2.50 7.70 0 -6 1 -0.30 4.10 0 6 -1 3.50 4.40 0 6 1 1.40 5.50 0 6 -1 -12.00 3.90 0 6 1 2.30 5.80 0 -6 -1 -2.50 3.50 0 6 1 -4.10 4.30 0 6 -1 -9.40 10.70 0 -6 -1 -2.00 3.80 0 6 -1 1.70 3.60 0 -6 1 5.00 6.30 0 -6 1 -1.50 3.20 0 -6 -1 2.60 5.90 0 -6 1 -0.30 6.20 0 -7 -1 114.39 12.60 0 -7 -1 117.19 13.30 0 -7 1 86.99 12.40 0 -7 1 108.19 12.40 0 7 1 94.09 9.20 0 7 -1 109.49 9.60 0 -7 -1 109.39 9.00 0 -7 1 93.29 9.40 0 7 -1 88.49 7.50 0 7 1 86.79 11.60 0 -7 -1 86.79 8.70 0 7 -1 75.39 11.30 0 -7 1 97.79 7.60 0 -8 -1 2.70 4.30 0 8 -1 -9.20 5.90 0 -8 1 -1.20 8.40 0 8 1 -14.50 6.60 0 -8 -1 -1.30 4.50 0 -8 1 7.30 7.70 0 8 -1 -5.20 8.60 0 -8 -1 -1.10 7.70 0 8 -1 -0.90 4.40 0 -8 -1 -0.90 7.50 0 -8 1 -0.10 3.60 0 8 -1 -2.00 3.60 0 8 1 -4.10 6.30 0 8 1 3.00 4.80 0 0 2 363.96 7.30 0 0 -2 348.77 7.40 0 0 -2 357.86 8.40 0 0 2 360.96 9.40 0 0 -2 345.67 9.20 0 0 -2 365.36 9.10 0 1 -2 4.20 1.90 0 1 -2 2.90 3.00 0 1 2 4.30 1.60 0 1 2 2.60 2.60 0 1 -2 1.20 1.50 0 1 2 5.70 3.70 0 -1 -2 0.20 1.70 0 -1 -2 8.40 3.40 0 -1 2 0.80 1.50 0 -1 2 1.70 2.20 0 -1 2 3.80 3.10 0 -1 2 3.60 3.30 0 -1 -2 -0.90 2.60 0 -1 -2 1.50 2.70 0 1 2 0.30 2.70 0 -2 2 2538.25 45.30 0 -2 -2 2573.34 48.60 0 -2 -2 2591.14 47.90 0 -2 -2 2601.14 49.60 0 -2 2 2529.25 47.90 0 2 -2 2559.44 47.90 0 -2 2 2438.86 49.30 0 2 2 2535.85 47.80 0 2 2 2561.54 48.60 0 2 -2 2435.86 52.19 0 2 -2 2498.85 44.90 0 2 2 2537.05 50.19 0 -3 -2 -0.50 3.70 0 3 -2 5.90 3.40 0 -3 -2 1.70 3.90 0 -3 -2 0.70 2.50 0 -3 2 1.40 2.10 0 3 2 -3.80 3.50 0 -3 2 -3.80 3.30 0 -3 -2 -1.10 3.80 0 3 -2 0.50 4.30 0 3 2 -0.70 4.00 0 -3 2 3.30 4.10 0 4 2 14.00 4.90 0 4 -2 15.30 4.80 0 -4 -2 12.70 3.50 0 -4 -2 14.20 5.50 0 4 -2 25.60 4.90 0 4 -2 18.00 3.00 0 -4 2 15.20 4.40 0 -4 -2 18.80 5.30 0 -4 -2 17.80 4.80 0 -4 2 17.60 5.50 0 4 -2 27.40 6.20 0 -4 2 19.80 3.00 0 4 2 30.30 6.20 0 -5 -2 3.10 5.40 0 5 -2 6.30 4.90 0 -5 2 -1.00 3.90 0 -5 2 -0.20 4.60 0 5 2 -0.70 5.30 0 5 -2 1.60 3.90 0 5 2 1.40 4.70 0 -5 2 -2.10 3.30 0 -5 -2 5.60 5.20 0 5 -2 4.60 5.60 0 5 -2 0.50 2.50 0 -5 -2 1.70 3.10 0 -5 -2 -1.60 4.50 0 6 2 96.89 10.00 0 6 -2 91.19 6.30 0 -6 2 86.59 6.40 0 -6 -2 72.79 9.40 0 6 2 105.99 11.80 0 -6 2 98.39 9.30 0 6 -2 98.79 9.10 0 -6 2 95.99 10.40 0 6 -2 94.09 11.70 0 6 2 87.29 10.00 0 -6 2 84.69 10.60 0 -6 -2 85.99 10.70 0 6 -2 96.79 10.30 0 -6 -2 81.89 7.60 0 7 -2 -11.60 5.20 0 -7 -2 -1.60 4.00 0 7 2 3.90 5.60 0 -7 -2 -15.10 5.00 0 7 2 4.90 6.60 0 -7 -2 -4.00 6.20 0 -7 2 -7.70 5.50 0 -7 -2 4.50 4.90 0 7 -2 -3.20 4.70 0 -7 2 7.60 3.70 0 7 2 -6.90 5.70 0 -7 2 -3.70 4.70 0 -7 2 -1.50 7.00 0 7 -2 -4.50 7.00 0 -8 2 18.80 6.30 0 8 2 17.90 9.60 0 8 -2 15.80 6.10 0 -8 -2 20.80 9.80 0 -8 2 18.50 9.20 0 8 -2 3.00 8.80 0 8 -2 29.50 8.40 0 8 2 11.20 7.30 0 -8 -2 19.70 9.30 0 8 2 22.00 6.30 0 -8 -2 23.00 5.70 0 -8 -2 20.70 6.50 0 0 -3 0.20 3.50 0 0 -3 8.30 6.50 0 0 3 4.10 3.60 0 0 3 1.20 1.80 0 0 -3 -1.70 2.80 0 0 -3 0.30 1.90 0 -1 -3 23.00 3.40 0 -1 3 20.90 3.50 0 -1 -3 17.90 4.40 0 1 -3 13.20 2.10 0 1 3 16.50 4.10 0 1 -3 16.00 3.20 0 1 -3 11.90 3.60 0 -1 -3 19.00 2.50 0 1 -3 19.30 2.00 0 1 3 14.60 3.60 0 1 3 16.30 3.10 0 -1 3 16.70 4.00 0 -1 -3 16.00 1.70 0 2 3 5.10 3.20 0 2 3 3.60 2.00 0 2 -3 0.70 4.00 0 -2 3 0.70 2.00 0 -2 3 0.80 3.50 0 -2 3 0.80 3.80 0 -2 3 -0.60 2.70 0 2 -3 0.50 3.30 0 -3 -3 170.58 9.10 0 3 -3 165.68 11.10 0 -3 3 185.78 11.10 0 3 -3 183.18 9.10 0 -3 3 181.98 7.20 0 3 -3 172.58 5.80 0 -3 3 188.58 9.50 0 3 3 180.38 9.90 0 3 3 159.58 11.00 0 -3 -3 185.78 9.80 0 -3 3 179.48 6.20 0 3 3 168.88 8.60 0 4 -3 0.00 3.70 0 4 3 0.30 4.00 0 4 -3 -0.10 5.00 0 -4 3 1.30 4.30 0 -4 -3 2.80 2.90 0 -4 3 -2.20 3.80 0 -4 -3 1.70 5.00 0 4 3 -2.90 4.20 0 -4 -3 1.90 4.00 0 -4 -3 -1.00 4.00 0 4 -3 -4.40 3.80 0 5 3 14.10 6.10 0 5 -3 21.20 5.80 0 5 -3 12.70 6.90 0 5 -3 16.70 5.20 0 -5 3 11.80 9.80 0 -5 3 19.50 5.50 0 -5 -3 22.10 6.30 0 6 3 7.80 6.80 0 6 3 0.40 5.60 0 -6 -3 -6.90 5.20 0 -6 -3 0.40 6.10 0 6 -3 4.70 7.00 0 -6 3 -3.70 4.80 0 -6 3 -2.50 4.80 0 -6 -3 -0.90 3.70 0 6 -3 -1.00 5.30 0 6 -3 7.80 5.20 0 -7 3 -4.30 5.10 0 -7 -3 -2.70 6.10 0 -7 -3 4.40 4.20 0 7 3 -0.50 6.00 0 7 3 -1.30 7.00 0 -7 3 0.40 6.90 0 -7 3 5.60 5.20 0 7 -3 0.50 7.50 0 -7 3 3.50 6.30 0 7 -3 -0.30 6.20 0 7 3 -2.90 5.80 0 7 -3 -0.70 5.00 0 8 -3 6.90 6.80 0 -8 -3 4.80 5.50 0 -8 3 0.90 7.20 0 -8 3 -1.90 5.30 0 -8 -3 2.70 7.50 0 -8 -3 2.90 4.40 0 8 -3 -0.60 4.80 0 8 -3 -7.90 9.10 0 -8 3 -10.70 4.60 0 8 3 12.60 6.50 0 8 3 -6.80 7.00 0 8 3 -6.10 6.10 0 -8 3 6.20 5.60 0 -8 -3 -9.50 10.10 0 0 -4 348.37 8.40 0 0 -4 351.36 11.30 0 0 -4 360.66 10.30 0 0 -4 345.47 11.50 0 0 4 352.56 11.90 0 0 4 344.97 8.90 0 -1 4 1.10 3.00 0 1 -4 -1.00 3.50 0 -1 4 -0.90 1.80 0 -1 4 3.30 4.00 0 1 4 -0.20 2.90 0 1 4 -2.80 3.60 0 -1 -4 -0.80 2.60 0 -1 -4 -0.50 2.20 0 -1 -4 0.60 1.50 0 -1 -4 -0.60 4.00 0 1 -4 2.20 3.00 0 2 4 939.71 22.60 0 2 -4 904.91 19.10 0 -2 4 922.71 23.80 0 -2 -4 933.91 24.20 0 -2 4 933.61 21.40 0 -2 4 932.91 22.80 0 2 4 897.31 18.70 0 2 4 888.81 23.80 0 2 4 942.81 21.50 0 2 -4 924.41 22.60 0 -2 -4 939.31 21.50 0 -3 -4 3.20 4.00 0 -3 -4 9.50 5.50 0 -3 4 -4.30 4.60 0 3 -4 -1.00 3.80 0 3 4 -0.70 2.80 0 3 -4 0.10 2.00 0 3 4 3.40 4.00 0 -3 4 1.70 4.10 0 -3 4 2.40 2.30 0 -3 4 1.20 3.00 0 -3 -4 0.50 3.60 0 3 4 0.10 3.70 0 -3 4 0.60 2.20 0 3 -4 3.90 5.10 0 -4 -4 421.46 15.50 0 4 -4 407.66 15.20 0 -4 -4 414.46 17.50 0 -4 4 410.16 12.30 0 4 4 407.36 16.10 0 4 -4 405.16 10.60 0 4 -4 402.36 17.50 0 -4 4 409.76 15.40 0 -4 4 416.86 17.30 0 -4 -4 398.56 15.90 0 4 4 435.76 17.70 0 -4 4 412.66 10.70 0 4 4 397.76 14.80 0 -4 -4 448.06 13.20 0 -5 4 -0.60 3.50 0 -5 4 -0.10 4.60 0 5 4 1.40 4.90 0 -5 -4 11.00 7.90 0 -5 -4 5.40 5.00 0 5 -4 -1.90 5.30 0 5 4 2.60 5.90 0 -5 -4 4.60 3.50 0 -5 4 6.60 5.30 0 5 -4 -2.50 4.20 0 -5 -4 -3.60 4.90 0 5 -4 12.50 7.50 0 6 -4 57.19 8.10 0 -6 -4 57.99 9.00 0 6 -4 75.59 11.70 0 -6 -4 51.09 6.20 0 -6 4 56.19 6.90 0 6 4 67.09 8.90 0 -6 4 67.89 8.70 0 -6 -4 58.09 9.50 0 -6 -4 73.89 11.20 0 6 -4 58.19 8.90 0 7 4 7.60 6.40 0 -7 -4 -2.50 7.10 0 7 -4 -0.40 5.80 0 7 -4 -3.30 5.30 0 -7 -4 8.50 6.90 0 -7 -4 -0.20 3.70 0 7 -4 -7.50 7.30 0 -7 4 1.60 9.70 0 -7 4 7.30 5.10 0 -7 4 0.00 5.50 0 7 4 7.40 7.60 0 8 4 78.69 11.70 0 8 4 73.49 12.00 0 8 -4 74.69 14.10 0 -8 4 86.49 9.80 0 -8 4 85.49 17.20 0 -8 -4 68.79 7.40 0 8 -4 85.69 10.40 0 -8 -4 86.29 13.20 0 -8 4 69.89 10.00 0 -8 4 75.69 10.30 0 8 -4 62.99 11.00 0 -8 -4 72.29 12.30 0 8 4 68.49 10.60 0 0 5 0.40 2.30 0 0 -5 1.50 3.80 0 0 -5 0.00 2.00 0 0 5 -1.50 3.50 0 0 -5 1.70 3.80 0 0 -5 -5.90 2.70 0 1 -5 257.87 10.90 0 -1 5 247.18 10.90 0 -1 -5 252.47 11.50 0 -1 -5 240.08 13.50 0 1 -5 251.67 10.30 0 -1 5 246.38 7.20 0 1 5 257.07 9.40 0 1 5 240.88 7.30 0 -1 -5 234.38 8.00 0 -1 5 235.48 9.90 0 1 5 241.88 11.50 0 -2 5 8.90 4.80 0 2 -5 -1.30 2.00 0 2 5 -7.10 3.20 0 -2 -5 1.80 1.70 0 -2 5 -1.20 4.50 0 2 5 1.40 4.90 0 2 5 5.30 3.50 0 -2 -5 4.00 4.60 0 -2 -5 -0.90 2.20 0 2 -5 -1.30 3.70 0 2 -5 -1.00 1.80 0 -2 5 0.50 3.20 0 -2 -5 2.60 3.50 0 3 5 126.79 8.40 0 3 5 122.39 9.10 0 -3 5 124.19 7.80 0 3 -5 130.09 8.90 0 -3 -5 112.39 9.90 0 3 5 110.69 5.70 0 3 -5 117.29 6.30 0 -3 -5 115.49 8.40 0 3 5 133.19 10.70 0 -3 5 140.69 9.50 0 -3 5 118.79 10.80 0 -4 5 -1.70 3.20 0 4 5 0.60 2.20 0 4 -5 0.30 4.20 0 -4 5 1.30 2.50 0 4 5 1.50 4.30 0 -4 -5 -0.60 4.10 0 -4 -5 -2.20 4.50 0 -4 5 1.30 5.00 0 4 -5 -0.40 2.10 0 4 5 -1.50 5.40 0 4 5 3.20 4.60 0 -4 -5 -1.90 4.40 0 -4 5 1.50 4.50 0 5 5 83.29 2.80 0 -5 -5 96.39 10.80 0 5 -5 89.09 9.10 0 -5 -5 106.59 10.40 0 -5 5 92.19 9.60 0 5 -5 101.39 19.10 0 5 5 88.09 6.20 0 5 5 88.19 9.20 0 -5 5 79.79 6.80 0 5 5 78.89 9.30 0 -5 -5 75.49 10.10 0 -5 -5 108.79 7.90 0 -5 5 87.69 4.90 0 -5 5 79.39 10.70 0 -6 -5 -7.10 4.60 0 6 5 -5.30 5.30 0 6 -5 -12.00 7.00 0 6 5 1.70 3.00 0 6 -5 -1.30 4.90 0 6 5 -4.70 5.50 0 -6 -5 4.90 6.10 0 6 -5 -2.10 4.70 0 -6 5 -4.20 9.80 0 -6 5 1.80 4.20 0 -6 -5 -2.80 3.60 0 -6 -5 10.70 6.00 0 7 -5 28.80 7.60 0 7 5 36.10 9.50 0 -7 -5 37.60 8.90 0 7 -5 63.69 11.90 0 -7 5 14.70 6.90 0 -7 5 28.00 6.30 0 7 5 45.10 9.20 0 7 -5 25.00 7.70 0 -7 -5 30.60 9.60 0 -7 -5 34.20 5.60 0 8 -5 9.00 6.30 0 -8 5 -6.30 3.70 0 8 5 6.70 8.80 0 -8 -5 8.90 9.00 0 8 5 -3.30 7.10 0 8 -5 -11.10 9.30 0 -8 -5 -5.30 3.20 0 8 5 2.40 2.80 0 -8 5 -5.80 5.40 0 8 5 3.50 7.60 0 -8 5 -3.20 5.30 0 0 6 51.99 6.40 0 0 -6 32.80 5.50 0 0 6 42.80 4.40 0 0 -6 45.90 6.20 0 0 -6 50.89 5.30 0 1 -6 4.40 2.60 0 -1 6 -2.10 3.60 0 -1 -6 2.40 3.10 0 -1 -6 0.40 4.30 0 -1 -6 2.50 2.80 0 -1 6 -0.50 2.00 0 1 -6 -3.80 4.20 0 1 6 -0.30 2.00 0 1 6 1.90 3.20 0 -1 -6 4.40 4.10 0 1 -6 7.20 3.90 0 2 -6 718.23 21.20 0 2 6 721.03 22.50 0 -2 -6 714.33 16.60 0 -2 6 744.43 20.00 0 2 6 755.32 20.90 0 -2 6 700.33 22.00 0 2 -6 695.33 15.40 0 -2 -6 733.13 14.80 0 -2 -6 718.73 22.60 0 2 6 738.03 19.30 0 -2 -6 722.33 19.10 0 -2 6 741.53 21.70 0 -3 -6 -3.60 4.00 0 -3 6 6.80 5.30 0 -3 6 -3.10 4.50 0 -3 -6 3.10 4.30 0 3 6 2.70 3.90 0 3 6 -0.30 5.40 0 3 -6 0.10 4.50 0 3 6 5.00 4.20 0 3 -6 0.80 2.60 0 -3 6 -1.70 3.30 0 -4 6 242.48 9.00 0 4 -6 251.87 13.60 0 4 -6 243.68 9.90 0 4 6 234.08 13.30 0 -4 -6 239.88 12.50 0 4 -6 230.48 8.10 0 4 6 256.37 12.60 0 -4 6 250.37 13.70 0 4 6 247.08 15.80 0 -4 6 232.08 11.50 0 -4 6 226.78 23.90 0 -4 -6 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6 -9 3.10 2.70 5 6 9 -6.60 10.00 5 -6 -9 3.30 8.40 5 0 -10 19.30 6.10 5 0 -10 19.10 7.40 5 0 10 23.80 8.10 5 0 10 15.20 5.00 -5 0 10 13.00 5.20 -5 0 -10 22.70 5.90 5 0 10 19.20 5.70 5 0 -10 24.20 6.80 5 0 10 15.70 1.80 -5 0 -10 11.30 7.40 -5 0 10 19.80 7.60 -5 0 10 14.10 2.60 -5 -1 -10 62.29 9.20 5 -1 10 41.20 7.00 5 1 -10 70.39 9.30 -5 -1 -10 52.59 8.60 -5 1 10 61.99 13.70 5 -1 10 56.79 7.90 5 1 -10 50.09 3.10 5 1 -10 51.59 5.00 5 -1 10 47.10 7.50 5 1 -10 66.69 7.40 5 1 -10 71.49 10.20 -5 1 10 54.09 6.30 -5 1 10 51.99 10.00 -5 -1 10 46.80 6.50 5 -1 -10 63.39 10.30 -5 -1 10 62.69 10.00 -5 1 -10 59.59 7.70 5 1 10 57.09 9.60 5 -1 -10 59.99 8.30 5 -1 -10 55.79 7.50 -5 1 -10 67.29 9.40 5 -2 10 3.20 5.60 -5 2 10 2.90 3.80 -5 2 10 -8.10 6.30 -5 -2 -10 2.00 1.40 5 2 -10 4.80 4.90 5 -2 10 4.30 5.40 -5 -2 -10 1.90 6.00 5 -2 10 7.50 5.20 -5 2 10 2.20 6.20 -5 -2 -10 -1.50 5.20 5 2 -10 4.50 3.10 5 2 10 -3.80 5.20 5 -2 -10 -3.90 7.20 5 2 10 3.40 3.60 -5 2 -10 4.90 4.00 -5 2 -10 2.30 1.70 -5 2 -10 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-2 157.88 14.50 12 -6 -2 191.78 19.90 12 6 2 162.28 14.40 12 -7 2 22.10 14.40 -12 7 2 26.70 9.80 -12 -7 -2 12.20 6.00 -12 -7 -2 4.40 7.50 -12 7 2 15.40 5.10 12 7 -2 2.10 6.80 12 -7 2 3.70 7.50 12 7 -2 20.50 7.40 -12 7 2 32.70 9.50 -12 -7 -2 8.70 7.80 12 -7 2 22.20 11.00 -12 7 -2 -0.10 8.10 -12 -7 2 9.90 7.80 12 -7 -2 20.30 7.00 -12 -7 2 1.10 2.70 12 7 2 7.80 4.00 12 7 2 13.60 7.50 12 -7 -2 10.20 8.00 -12 -7 2 16.70 8.10 12 -7 -2 17.20 8.40 12 7 2 24.00 9.60 -12 0 -3 285.77 12.00 12 0 -3 301.77 13.90 -12 0 3 304.37 12.40 -12 0 -3 280.57 8.60 12 0 3 305.47 14.20 -12 0 3 287.67 14.80 12 0 -3 260.67 11.60 -12 0 3 286.37 16.50 -12 0 -3 283.37 11.40 -12 0 3 265.97 12.40 -12 0 -3 303.47 20.90 12 0 3 268.57 13.80 -12 0 -3 292.67 16.10 -12 0 3 281.47 12.50 12 0 3 291.07 12.30 -12 0 3 254.87 15.60 -12 0 3 275.17 15.40 12 0 -3 259.27 13.30 -12 0 3 309.57 15.10 -12 0 3 277.17 8.80 12 0 -3 280.97 12.60 -12 0 -3 286.77 14.00 -12 0 -3 293.87 13.50 -12 0 -3 319.37 15.20 -12 -1 -3 287.07 14.40 -12 1 3 295.07 15.10 12 1 -3 265.97 13.50 -12 -1 -3 276.57 11.30 12 -1 3 265.67 13.80 12 1 -3 260.17 13.80 -12 -1 -3 229.78 20.10 -12 1 3 307.67 13.10 -12 1 3 305.37 9.50 12 -1 3 252.57 12.80 -12 1 3 297.57 11.00 12 1 -3 282.57 13.00 12 1 -3 282.47 13.70 -12 1 3 265.97 21.20 -12 1 3 303.37 14.70 -12 1 3 307.47 13.60 12 -1 3 268.97 14.10 -12 1 3 306.77 15.20 -12 1 3 293.97 16.40 -12 -1 -3 266.37 15.00 -12 1 3 311.67 17.00 12 1 3 268.77 13.30 12 -1 -3 300.47 13.60 -12 1 -3 273.67 13.90 -12 1 -3 282.27 11.60 12 -1 -3 284.97 13.50 -12 -1 3 275.17 16.60 -12 1 -3 259.27 15.70 -12 1 -3 292.27 13.60 -12 1 -3 270.97 10.50 12 1 3 260.47 14.90 -12 1 -3 264.47 10.90 12 1 3 269.77 12.20 12 -1 -3 297.67 14.10 -12 1 -3 262.67 11.40 -12 1 -3 305.67 16.60 -12 1 -3 282.47 16.90 -12 -1 3 271.97 11.80 -12 -1 3 306.77 13.60 -12 -1 3 296.87 20.70 -12 1 -3 246.68 12.30 -12 -1 3 277.67 14.70 -12 -1 3 301.67 18.40 12 1 3 281.77 14.00 12 1 3 255.07 11.00 -12 2 3 8.60 5.40 12 2 -3 5.00 5.60 12 -2 3 3.20 5.50 -12 2 3 7.50 5.00 12 -2 3 2.80 3.50 -12 2 3 5.20 4.90 -12 2 3 5.10 5.90 -12 -2 -3 14.60 5.80 -12 2 3 6.40 5.70 -12 -2 -3 12.80 5.90 -12 2 3 6.30 3.30 12 2 -3 -1.70 2.90 -12 2 3 -1.50 4.40 12 -2 3 0.50 5.40 12 2 -3 -8.40 4.50 12 2 -3 -4.70 5.00 -12 2 3 4.50 4.10 -12 -2 -3 10.90 5.50 -12 2 3 4.10 4.80 -12 2 3 4.20 5.10 -12 2 -3 0.20 4.90 12 2 3 -0.30 4.50 -12 2 -3 -1.00 4.80 -12 -2 3 2.80 5.40 -12 2 -3 7.90 4.10 -12 2 -3 7.80 4.30 -12 2 -3 9.20 5.20 -12 2 -3 5.70 4.90 12 2 3 5.10 4.30 -12 2 -3 4.80 2.00 12 2 3 8.80 6.60 -12 -2 3 2.80 4.60 12 2 3 2.90 5.00 -12 2 -3 0.20 3.60 12 -2 -3 5.80 5.20 -12 -2 3 5.60 5.70 -12 -2 3 2.40 3.80 12 -2 -3 6.60 5.40 -12 -2 3 -5.20 4.40 -12 -2 3 -1.50 4.90 -12 -2 3 2.70 3.40 12 -2 -3 3.40 4.70 12 3 -3 223.58 13.50 12 3 -3 245.08 11.00 -12 3 3 247.08 5.70 -12 -3 -3 273.17 15.00 12 -3 3 288.67 14.40 -12 3 3 246.98 12.40 12 3 -3 271.77 14.20 -12 3 3 252.67 14.10 -12 3 3 239.68 15.80 12 3 -3 260.47 14.50 12 3 -3 253.37 13.50 -12 -3 -3 258.37 15.00 -12 -3 -3 241.48 7.50 -12 3 3 235.18 13.90 12 -3 3 286.37 17.80 12 -3 3 259.47 13.70 -12 3 -3 252.27 13.90 -12 3 -3 250.57 13.80 -12 -3 3 230.58 22.10 12 -3 -3 253.37 12.10 -12 3 -3 271.07 11.80 12 -3 -3 251.37 14.30 -12 -3 3 256.27 11.30 -12 3 -3 259.97 11.60 -12 -3 3 274.47 11.50 12 3 3 238.88 11.90 12 3 3 240.38 13.20 12 -3 -3 242.38 13.20 12 3 3 262.57 16.00 -12 -3 3 261.77 15.60 -12 -3 3 246.08 15.00 -12 3 -3 260.97 14.30 12 -3 -3 280.87 15.00 -12 -3 3 247.28 15.40 12 3 3 237.68 13.50 12 -4 3 25.90 6.40 -12 4 3 12.60 6.00 12 4 -3 15.20 6.80 12 -4 3 25.80 7.60 12 4 -3 30.20 7.90 12 4 -3 23.60 5.50 12 -4 3 19.40 7.30 -12 4 3 23.30 7.80 -12 4 3 8.80 4.90 -12 4 3 12.10 4.90 -12 4 3 11.20 5.10 12 -4 3 25.10 7.00 12 4 -3 29.40 8.70 -12 -4 -3 22.20 3.90 -12 -4 -3 24.10 7.50 -12 -4 -3 25.50 7.40 12 4 3 17.70 6.70 -12 -4 3 23.90 5.80 12 4 3 20.30 6.60 12 4 3 18.40 3.70 12 4 3 19.40 5.70 12 -4 -3 20.90 5.40 -12 -4 3 18.60 7.10 -12 4 -3 20.50 6.40 -12 -4 3 9.60 5.50 -12 4 -3 24.50 7.50 -12 4 -3 32.10 6.00 12 4 3 30.60 8.80 -12 -4 3 8.80 7.50 12 -4 -3 19.60 6.00 -12 4 -3 16.10 4.80 12 -4 -3 22.00 7.30 12 -4 -3 13.90 6.80 -12 -4 3 16.80 7.20 12 5 -3 85.09 10.70 -12 -5 -3 89.59 11.40 -12 5 3 73.49 9.90 -12 -5 -3 94.39 11.40 -12 -5 -3 84.19 8.10 -12 5 3 82.39 9.00 12 -5 3 69.89 10.40 -12 5 3 80.79 11.60 -12 5 3 98.19 9.00 12 5 -3 96.79 12.10 -12 5 3 81.29 9.60 12 -5 3 83.39 11.60 12 -5 3 91.79 11.30 12 5 -3 81.09 9.10 -12 -5 3 71.49 10.60 12 5 3 106.89 13.10 12 -5 -3 90.79 11.00 -12 -5 3 97.09 9.60 12 5 3 80.29 10.50 12 5 3 94.49 6.10 12 5 3 80.99 10.40 -12 5 -3 102.09 12.70 -12 -5 3 72.39 10.30 -12 5 -3 80.49 7.40 12 -5 -3 75.29 10.30 12 -5 -3 71.89 8.60 -12 -5 3 71.49 10.60 12 -5 -3 71.59 14.10 12 -6 3 34.00 8.70 12 -6 3 17.50 6.10 -12 6 3 20.20 8.70 12 -6 3 26.10 8.90 -12 6 3 28.70 9.60 12 -6 3 24.90 9.70 12 6 -3 25.60 8.60 -12 -6 -3 41.10 9.10 12 6 -3 19.10 7.70 -12 -6 -3 31.00 8.60 -12 -6 -3 18.00 9.50 -12 -6 -3 21.60 5.30 -12 6 3 29.20 7.30 12 -6 -3 33.20 10.40 12 6 3 26.00 4.10 12 -6 -3 44.20 9.30 12 -6 -3 30.30 7.00 -12 -6 3 24.70 5.80 -12 -6 3 23.60 8.80 -12 -6 3 23.90 8.00 -12 -6 3 29.70 9.00 -12 6 -3 22.70 9.30 -12 6 -3 35.60 4.90 12 6 3 27.00 9.60 12 6 3 23.60 8.60 12 -6 -3 26.60 8.90 12 -6 -3 31.10 6.80 12 6 3 22.60 7.50 -12 -7 -3 77.29 12.00 12 -7 3 57.69 10.70 12 -7 3 60.59 17.30 -12 -7 -3 75.19 11.20 -12 7 3 44.60 11.70 12 -7 3 52.79 7.90 12 -7 3 44.90 10.40 -12 -7 -3 69.39 8.60 12 7 -3 79.19 10.90 12 7 -3 58.29 10.60 12 -7 -3 52.39 8.70 -12 7 -3 45.90 11.40 12 7 3 57.49 11.90 -12 7 -3 65.59 5.70 -12 -7 3 42.20 9.90 12 -7 -3 70.29 10.80 -12 -7 3 66.49 11.60 12 -7 -3 62.89 11.20 12 0 4 343.97 13.10 -12 0 -4 376.06 16.40 12 0 -4 357.66 13.90 12 0 -4 361.66 15.80 -12 0 -4 341.47 16.00 -12 0 4 369.66 17.30 12 0 -4 361.56 14.40 -12 0 4 372.56 16.10 -12 0 4 362.56 15.60 -12 0 4 369.46 14.30 -12 0 -4 363.86 15.90 12 0 -4 362.26 15.80 12 0 4 357.96 16.40 -12 0 -4 360.76 12.40 12 0 4 360.76 15.90 -12 0 4 356.26 17.00 -12 0 -4 361.06 8.10 -12 0 4 365.46 8.60 -12 0 -4 346.97 13.30 -12 0 4 373.46 14.10 12 -1 4 344.67 15.80 -12 1 4 386.16 19.00 -12 1 4 332.47 15.30 -12 1 4 336.77 12.30 -12 1 4 367.26 15.80 -12 1 4 325.07 15.00 -12 1 4 342.07 13.70 12 1 -4 336.17 12.90 -12 -1 -4 371.46 16.40 -12 -1 -4 379.76 16.30 -12 1 4 348.27 16.50 12 -1 4 353.56 15.10 12 1 -4 329.17 15.30 -12 1 4 334.27 16.90 12 1 -4 354.16 14.90 -12 1 4 345.47 8.80 -12 1 4 312.87 16.30 -12 -1 -4 333.77 12.00 12 -1 4 349.27 16.20 12 1 -4 350.56 15.60 -12 1 -4 337.77 12.30 -12 1 -4 354.26 16.30 -12 -1 4 358.46 14.70 -12 1 -4 316.97 15.70 12 1 4 323.37 16.50 12 -1 -4 337.17 15.60 12 1 4 342.67 13.70 12 -1 -4 340.17 15.70 -12 1 -4 344.57 12.70 -12 1 -4 350.86 11.70 -12 1 -4 316.47 10.80 -12 1 -4 324.07 15.70 -12 1 -4 330.77 13.90 12 1 4 360.26 12.10 12 -1 -4 348.87 14.40 12 -1 -4 319.97 14.50 -12 1 -4 347.17 15.20 -12 -1 4 328.17 12.70 -12 -1 4 336.27 9.30 -12 -1 4 348.47 17.10 -12 -1 4 356.66 16.30 12 -1 -4 345.57 12.20 -12 -1 4 362.76 17.10 12 1 4 329.17 16.00 12 1 4 336.37 15.20 12 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80.89 9.70 12 -3 4 79.99 8.40 -12 3 4 58.79 9.70 -12 3 4 83.99 6.80 -12 -3 -4 81.19 9.90 12 3 -4 79.59 11.30 12 3 4 79.19 9.10 -12 -3 4 74.39 7.10 -12 -3 4 93.39 10.40 -12 -3 4 111.29 12.50 -12 3 -4 75.59 8.10 12 3 4 104.59 10.50 12 -3 -4 87.19 10.00 12 3 4 75.69 7.60 12 3 4 72.39 8.70 -12 3 -4 86.89 10.20 -12 3 -4 61.49 6.30 -12 3 -4 90.89 10.20 12 3 4 64.19 10.80 12 -3 -4 62.79 9.00 -12 -3 4 82.89 10.80 -12 -3 4 73.69 7.10 -12 3 -4 81.99 8.90 12 -4 4 142.99 12.90 12 -4 4 142.99 12.00 -12 -4 -4 146.99 6.20 12 4 -4 141.49 12.10 12 4 -4 140.49 9.40 -12 4 4 144.39 9.30 -12 4 4 147.49 14.70 -12 4 4 152.78 10.60 -12 -4 -4 141.59 13.30 12 4 -4 141.19 12.20 -12 4 4 137.79 12.50 -12 -4 -4 133.29 12.50 12 4 -4 155.68 12.80 -12 -4 -4 137.59 15.00 -12 -4 4 144.79 13.60 12 -4 -4 148.69 11.80 12 4 4 130.89 12.00 -12 -4 4 148.49 15.00 -12 4 -4 141.99 13.00 -12 4 -4 127.69 8.80 12 4 4 156.88 10.50 -12 -4 4 122.09 8.20 12 -4 -4 135.89 12.20 12 -4 -4 149.19 12.90 -12 -4 4 149.29 13.30 12 4 4 137.69 13.60 -12 4 -4 135.89 10.20 -12 -4 4 156.28 13.00 12 -4 -4 148.29 9.90 -12 5 4 124.69 16.10 12 -5 4 140.19 13.40 12 5 -4 138.79 19.10 -12 -5 -4 145.39 14.30 12 5 -4 137.09 13.10 12 -5 4 130.89 11.70 -12 5 4 155.68 16.40 12 -5 4 155.08 13.30 -12 -5 -4 143.09 15.90 12 5 -4 151.78 10.80 12 5 -4 164.18 13.40 12 -5 4 125.69 13.70 -12 -5 -4 163.48 14.60 -12 5 4 156.18 16.40 -12 -5 -4 134.89 8.10 -12 5 4 142.79 12.60 -12 5 4 139.39 9.90 -12 -5 4 156.68 14.10 -12 -5 4 135.59 14.30 -12 5 -4 153.88 10.20 12 -5 -4 156.98 14.20 12 -5 -4 146.09 10.10 12 5 4 135.59 14.40 12 -5 -4 161.58 12.40 12 5 4 140.09 13.50 12 5 4 158.68 14.00 12 -5 -4 138.39 12.90 -12 5 -4 134.09 14.80 -12 -6 -4 39.80 9.30 12 -6 4 27.50 6.70 -12 -6 -4 18.60 8.80 12 6 -4 35.80 10.00 -12 6 4 32.00 8.00 12 6 -4 32.80 8.90 12 -6 4 38.20 9.30 12 -6 4 32.00 10.00 -12 6 4 28.70 8.20 12 6 -4 27.40 8.40 -12 6 4 28.90 6.90 -12 -6 -4 22.50 5.00 12 -6 4 24.90 8.90 -12 6 4 38.40 11.40 -12 -6 -4 8.70 9.30 -12 -6 4 27.80 8.70 -12 -6 4 32.90 10.20 12 -6 -4 31.70 8.70 12 6 4 15.10 7.80 12 -6 -4 38.50 7.20 12 6 4 28.90 9.70 -12 6 -4 24.70 9.30 -12 -6 4 36.10 9.70 12 -6 -4 33.70 9.60 -12 6 -4 36.20 7.90 12 -6 -4 10.00 5.50 -12 6 -4 38.30 5.90 12 0 -5 147.49 11.50 -12 0 -5 128.19 11.30 12 0 -5 123.39 11.10 12 0 -5 139.39 9.90 -12 0 -5 144.09 8.70 -12 0 5 141.99 11.00 -12 0 -5 147.19 12.10 12 0 5 127.49 11.50 -12 0 5 136.59 11.10 -12 0 5 135.89 9.30 12 0 -5 122.19 9.40 -12 0 5 142.69 9.80 -12 0 5 127.49 12.40 -12 0 -5 121.09 10.70 12 0 5 120.19 11.00 -12 0 -5 121.49 8.70 12 0 5 140.39 8.40 -12 0 5 128.49 11.70 -12 -1 -5 284.27 10.80 12 -1 5 269.17 9.40 -12 1 5 303.27 15.00 -12 1 5 298.67 14.80 -12 -1 -5 281.87 17.10 -12 1 5 294.87 12.30 12 -1 5 293.27 14.30 -12 1 5 286.37 16.00 12 -1 5 298.67 18.60 -12 1 5 285.67 11.70 -12 -1 -5 285.27 14.90 -12 -1 -5 277.27 13.60 12 1 -5 271.97 21.90 12 1 -5 271.77 11.80 12 1 -5 267.87 13.40 -12 1 5 281.97 16.40 -12 -1 5 277.17 16.00 12 -1 -5 280.67 11.40 12 -1 -5 294.97 13.30 12 1 5 296.07 15.00 12 1 5 266.97 15.30 -12 1 -5 282.47 9.80 -12 1 -5 294.07 15.40 -12 1 -5 279.57 9.80 12 1 5 286.37 12.30 12 -1 -5 274.27 14.90 -12 1 -5 280.37 14.80 -12 -1 5 266.47 16.30 -12 1 -5 299.37 16.20 12 -1 -5 305.37 14.40 -12 1 -5 279.67 10.90 -12 -1 5 275.37 14.10 -12 -1 5 263.37 14.90 12 1 5 287.77 15.00 12 -2 5 81.09 7.40 -12 2 5 80.99 11.00 -12 2 5 79.69 10.30 -12 2 5 89.99 9.80 -12 2 5 67.89 4.00 -12 -2 -5 65.69 9.00 12 -2 5 64.99 8.80 -12 2 5 73.89 9.10 12 -2 5 79.89 8.50 -12 -2 -5 74.69 10.10 -12 2 5 65.49 4.10 12 2 -5 76.79 9.50 -12 2 5 82.99 9.20 12 2 -5 57.59 4.60 12 2 -5 79.99 9.60 12 2 -5 57.59 8.00 -12 2 5 65.69 5.90 -12 -2 -5 81.19 9.80 12 -2 5 76.19 10.00 12 2 -5 58.89 8.70 -12 2 -5 66.69 9.10 12 2 5 67.99 6.40 -12 -2 5 62.89 6.40 12 -2 -5 61.89 8.70 -12 2 -5 73.29 6.90 -12 -2 5 65.89 9.10 -12 -2 5 89.69 11.40 12 2 5 74.79 8.10 -12 2 -5 70.49 8.00 -12 -2 5 70.19 10.10 -12 2 -5 76.29 9.70 12 2 5 62.99 10.00 -12 2 -5 60.99 6.00 12 2 5 71.29 8.90 -12 -2 5 70.89 9.00 12 -2 -5 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-19 -2 -5 23.70 7.90 -19 2 5 33.60 2.80 -19 2 5 19.40 8.60 -19 2 5 49.20 11.50 19 2 -5 41.30 9.30 19 -2 5 38.20 10.00 -19 -2 -5 35.70 9.20 -19 -2 5 43.30 9.50 -19 -2 5 39.60 10.30 -19 2 -5 32.30 5.90 -19 2 -5 57.79 16.60 -19 2 -5 40.10 10.60 -19 2 -5 47.00 7.40 -19 -2 5 35.20 8.40 19 2 5 26.80 9.90 -19 2 -5 21.40 6.80 19 -2 -5 26.70 13.20 19 2 5 24.20 7.20 19 0 -6 7.70 7.60 -19 0 6 10.10 5.50 -19 0 -6 -6.60 4.40 -19 0 -6 10.10 4.20 -19 0 -6 9.70 7.80 -19 0 6 4.20 5.50 19 0 6 -0.50 6.40 -19 0 -6 7.60 5.60 -19 0 6 10.10 7.80 -19 0 -6 -1.70 7.60 19 0 6 13.40 8.30 -19 1 6 101.09 15.60 -19 1 6 107.99 15.40 19 1 -6 115.99 13.80 -19 1 6 115.59 11.90 19 -1 6 101.09 13.20 -19 1 6 70.39 17.30 -19 -1 -6 100.89 13.50 19 -1 6 117.79 13.70 -19 -1 -6 127.29 14.10 -19 -1 -6 110.69 11.50 -19 -1 6 119.89 12.40 19 1 6 95.19 12.30 19 -1 -6 108.29 12.40 -19 1 -6 123.29 11.20 -19 1 -6 105.09 13.40 -19 -1 6 117.29 14.80 -19 1 -6 106.39 7.20 -19 -1 6 103.39 11.50 -19 1 -6 94.69 7.00 -20 0 0 3.10 5.60 -20 0 0 0.20 4.50 -20 0 0 -4.00 4.30 -20 0 0 8.10 5.00 -20 0 0 0.60 5.70 -20 0 0 6.50 5.60 -20 0 0 -4.10 6.40 -20 0 0 -5.00 5.10 -20 0 0 2.20 5.30 -20 0 0 17.90 7.40 -20 -1 0 23.20 5.70 -20 -1 0 29.40 9.20 -20 1 0 18.20 6.40 -20 -1 0 24.30 7.00 -20 -1 0 26.90 7.90 -20 -1 0 17.00 8.10 -20 -1 0 24.00 7.50 -20 1 0 22.10 5.80 -20 1 0 13.70 7.80 -20 1 0 32.00 7.80 -20 1 0 27.00 7.20 -20 1 0 38.30 8.80 -20 -1 0 28.60 7.60 -20 1 0 27.10 6.70 -20 1 0 25.10 7.80 -20 1 0 25.80 6.10 -20 -1 0 39.20 9.20 -20 1 0 41.10 9.10 -20 -1 0 20.30 6.20 -20 1 0 35.30 9.70 -20 2 0 25.00 6.30 -20 2 0 25.10 5.80 20 2 0 22.00 12.80 -20 -2 0 35.30 7.30 -20 2 0 49.70 9.30 -20 -2 0 18.10 8.30 -20 2 0 37.40 7.40 -20 2 0 33.00 10.30 -20 -2 0 31.60 5.70 -20 -2 0 28.00 6.80 -20 2 0 17.90 7.90 -20 2 0 29.30 6.80 20 2 0 20.50 7.70 -20 -2 0 23.20 8.10 -20 2 0 23.80 9.50 -20 2 0 32.10 8.20 -20 -2 0 26.80 6.20 -20 2 0 17.60 7.30 -20 -2 0 26.30 8.60 -20 2 0 23.40 7.60 -20 -3 0 31.20 8.70 -20 -3 0 30.60 8.90 -20 3 0 44.60 8.30 -20 3 0 25.00 7.00 -20 3 0 40.50 8.70 20 3 0 22.90 8.50 20 3 0 32.80 6.90 -20 3 0 22.00 5.80 -20 3 0 27.70 6.60 -20 -3 0 22.50 6.30 -20 -3 0 31.70 5.80 -20 -3 0 43.80 8.10 -20 -3 0 46.20 7.50 -20 3 0 25.60 5.20 -20 -3 0 32.00 14.30 -20 0 -1 28.20 8.20 -20 0 -1 24.30 8.60 -20 0 1 22.10 8.40 -20 0 1 20.00 7.40 -20 0 1 24.00 6.40 -20 0 -1 37.20 9.60 -20 0 -1 34.90 7.30 -20 0 1 40.40 10.50 -20 0 1 13.00 6.70 -20 0 -1 23.20 7.20 -20 0 -1 18.90 7.50 -20 0 -1 23.50 6.80 -20 0 -1 9.60 7.80 -20 0 -1 9.40 4.60 -20 0 1 23.40 5.70 -20 0 1 19.70 6.60 -20 0 -1 15.70 5.70 -20 0 1 29.10 9.00 -20 0 1 27.70 11.00 -20 -1 -1 11.20 4.50 -20 -1 -1 13.10 6.60 -20 1 1 16.50 7.40 -20 1 1 11.70 5.60 -20 1 1 8.90 7.50 -20 1 1 9.40 4.90 -20 1 1 7.60 4.70 -20 1 1 3.20 6.00 -20 -1 -1 13.80 6.10 -20 1 1 3.20 6.10 -20 1 1 8.30 6.30 -20 1 1 -3.40 6.30 -20 -1 -1 6.30 6.10 -20 -1 -1 1.20 6.90 -20 -1 -1 4.50 7.40 -20 -1 -1 23.20 8.40 -20 -1 -1 20.20 6.80 -20 1 1 9.50 5.60 -20 1 1 13.60 6.80 -20 1 1 9.10 6.60 -20 -1 1 12.20 6.40 -20 -1 1 5.00 6.40 -20 -1 1 6.00 12.00 -20 1 -1 14.40 7.60 -20 -1 1 13.20 7.60 -20 1 -1 9.00 6.40 -20 1 -1 10.00 6.70 -20 -1 1 10.90 7.20 -20 1 -1 15.20 5.70 -20 1 -1 7.80 5.80 -20 1 -1 3.80 4.60 -20 1 -1 10.90 7.60 -20 -1 1 9.50 7.90 -20 -1 1 4.40 7.10 -20 -1 1 15.30 5.60 -20 1 -1 15.30 6.70 -20 1 -1 -1.70 9.60 -20 1 -1 26.50 8.40 -20 -1 1 14.20 8.50 -20 1 -1 7.60 5.30 -20 2 1 95.49 9.00 -20 -2 -1 88.79 11.70 20 2 -1 124.09 12.80 20 2 -1 104.99 15.60 -20 2 1 109.69 13.30 -20 2 1 112.79 20.00 -20 2 1 108.19 11.80 -20 2 1 95.09 13.50 -20 -2 -1 101.59 8.30 -20 2 1 89.19 12.30 -20 -2 -1 109.09 12.50 -20 2 1 102.49 10.70 -20 2 1 131.59 12.90 -20 2 1 92.09 9.50 -20 -2 -1 109.99 11.60 -20 -2 -1 87.49 8.50 -20 2 1 105.09 12.50 -20 -2 -1 108.29 12.80 -20 -2 -1 101.69 10.90 -20 -2 1 121.99 14.80 -20 -2 1 107.39 15.30 -20 -2 1 110.99 13.40 -20 -2 1 121.69 11.20 -20 -2 1 103.79 10.30 20 2 1 117.29 12.10 -20 2 -1 123.99 12.30 -20 2 -1 106.49 10.90 -20 2 -1 115.79 11.40 -20 2 -1 108.49 9.80 -20 2 -1 101.79 12.10 -20 -2 1 106.99 12.40 -20 2 -1 129.69 12.30 -20 2 -1 110.39 13.70 -20 -2 1 105.99 10.60 -20 2 -1 107.39 12.00 20 2 1 114.69 13.00 -20 -3 -1 0.20 7.40 20 3 -1 37.90 9.50 -20 -3 -1 30.90 7.80 -20 3 1 6.00 6.30 -20 3 1 8.60 5.20 20 3 -1 8.50 7.00 20 3 -1 11.40 6.70 -20 3 1 13.00 4.00 -20 -3 -1 13.80 4.50 -20 -3 -1 16.00 4.50 -20 3 1 19.70 5.60 -20 -3 -1 14.80 7.40 -20 3 1 17.00 8.80 -20 -3 -1 27.40 6.50 -20 3 1 28.70 8.00 20 3 1 11.80 7.10 -20 -3 1 15.40 8.10 -20 3 -1 11.50 6.30 -20 3 -1 23.30 6.60 -20 3 -1 11.80 7.40 -20 3 -1 14.20 4.70 -20 -3 1 -1.70 5.60 -20 3 -1 14.90 6.10 20 3 1 6.50 5.60 -20 -3 1 23.70 8.50 20 3 1 14.80 7.40 -20 3 -1 4.40 4.20 -20 -3 1 31.10 6.40 -20 -3 1 7.90 5.30 -20 3 -1 17.30 6.80 -20 0 -2 18.70 7.10 -20 0 -2 22.40 7.20 -20 0 2 18.40 13.60 -20 0 -2 28.70 7.70 -20 0 2 17.10 6.80 -20 0 -2 27.00 7.60 -20 0 2 23.70 9.60 -20 0 2 20.00 7.20 -20 0 -2 29.30 9.70 -20 0 2 12.90 4.90 -20 0 -2 24.50 8.90 -20 0 2 19.10 8.20 -20 0 2 11.60 5.50 -20 0 2 22.30 6.60 -20 0 -2 14.50 7.30 -20 0 2 14.40 7.80 -20 0 -2 24.80 8.40 -20 0 -2 17.40 4.60 -20 -1 -2 188.58 14.70 -20 1 2 185.98 15.20 -20 1 2 149.59 10.20 -20 1 2 198.78 15.00 -20 -1 -2 156.08 13.90 -20 -1 -2 180.38 13.50 -20 -1 -2 186.38 8.80 -20 -1 -2 180.68 14.30 -20 1 2 201.38 12.40 -20 1 2 163.08 13.40 -20 1 2 186.58 15.10 -20 -1 -2 191.38 14.10 -20 -1 -2 149.39 8.20 -20 -1 -2 167.08 17.60 -20 1 2 168.78 14.80 -20 1 2 192.88 15.40 -20 1 2 185.28 14.00 -20 1 2 171.28 20.30 -20 -1 2 165.68 15.20 -20 -1 2 152.68 12.90 -20 -1 2 186.08 15.80 -20 -1 2 178.28 13.10 -20 1 -2 175.08 16.90 -20 -1 2 192.38 14.80 -20 1 -2 180.88 14.20 -20 1 -2 176.08 12.40 -20 1 -2 214.48 19.00 -20 1 -2 185.98 13.70 -20 -1 2 176.68 14.20 -20 -1 2 174.38 14.30 -20 1 -2 177.18 12.00 -20 1 -2 165.88 10.90 -20 1 -2 179.18 16.50 -20 -1 2 204.08 19.00 -20 1 -2 196.68 14.60 -20 1 -2 166.28 13.30 -20 -1 2 171.28 10.70 -20 2 2 36.30 9.10 -20 2 2 47.20 9.10 -20 -2 -2 40.70 8.50 -20 2 2 43.60 7.80 20 2 -2 37.80 8.80 20 2 -2 44.50 10.90 -20 2 2 38.30 9.70 -20 -2 -2 34.10 3.60 -20 2 2 34.30 5.80 -20 -2 -2 54.79 12.50 -20 -2 -2 43.10 9.10 -20 2 2 57.09 13.40 -20 -2 -2 53.89 9.50 -20 2 2 63.09 10.60 -20 -2 -2 47.10 9.20 -20 2 2 30.80 5.80 -20 2 -2 54.99 9.90 -20 -2 2 33.60 7.60 -20 2 -2 44.10 8.70 -20 -2 2 46.50 10.10 -20 2 -2 47.30 7.10 -20 2 -2 42.90 6.30 20 2 2 52.59 9.70 -20 2 -2 54.19 9.40 -20 -2 2 48.30 9.60 -20 -2 2 22.90 6.30 -20 2 -2 30.70 6.70 -20 -2 2 37.60 8.60 20 2 2 40.90 10.70 -20 -2 2 37.40 8.90 -20 -2 2 45.50 6.60 -20 2 -2 46.90 9.10 -20 0 -3 41.10 9.30 -20 0 -3 40.70 8.70 -20 0 -3 43.60 8.90 -20 0 3 38.20 10.50 -20 0 -3 28.50 11.40 -20 0 3 32.00 5.10 -20 0 3 33.80 9.00 -20 0 -3 29.60 7.80 -20 0 -3 34.10 6.70 -20 0 3 52.29 11.10 -20 0 3 31.40 9.10 -20 0 3 38.20 7.20 -20 0 3 47.70 7.90 -20 0 3 45.60 16.50 -20 1 3 8.60 10.50 -20 -1 -3 15.60 6.80 -20 -1 -3 -6.90 9.00 -20 1 3 4.10 3.70 -20 1 3 13.90 6.40 -20 -1 -3 13.60 5.50 20 1 -3 10.70 7.30 -20 1 3 18.80 7.00 -20 -1 -3 13.80 7.40 -20 1 3 15.50 6.70 -20 1 3 25.10 8.40 -20 -1 -3 10.70 7.00 -20 1 -3 14.50 4.90 -20 -1 3 4.90 6.80 -20 -1 3 11.10 3.90 -20 1 -3 5.40 4.20 -20 -1 3 17.70 7.30 -20 -1 3 14.60 7.80 -20 1 -3 13.40 6.40 -20 1 -3 10.20 10.10 -20 1 -3 14.10 5.70 -20 -1 3 6.20 5.10 20 1 3 9.60 10.10 -20 1 -3 -3.60 7.90 -20 -1 3 14.70 7.20 -20 1 -3 12.20 7.20 -20 2 3 112.09 8.30 -20 -2 -3 99.49 12.30 -20 -2 -3 102.89 13.30 -20 2 3 117.69 13.10 -20 2 3 91.69 8.10 -20 2 3 146.09 14.00 -20 2 3 121.09 20.30 -20 -2 -3 128.39 13.40 20 2 -3 103.59 12.50 20 2 -3 134.29 16.90 -20 2 3 92.89 11.90 -20 2 -3 96.39 12.30 -20 -2 3 103.19 8.80 20 2 3 125.29 13.20 -20 2 -3 97.99 13.50 -20 2 -3 121.89 13.30 -20 2 -3 111.59 11.80 -20 2 -3 101.39 9.90 -20 2 -3 114.89 11.50 -20 -2 3 100.59 10.90 -20 2 -3 98.29 9.60 -20 -2 3 118.09 13.10 20 2 3 121.79 15.40 -20 2 -3 114.79 8.10 -20 -2 3 114.99 12.10 -20 -2 3 101.39 12.60 -20 0 4 -4.80 2.60 -20 0 4 -5.70 5.10 -20 0 4 9.10 7.20 -20 0 -4 -3.70 4.40 -20 0 -4 4.60 6.80 -20 0 4 7.40 5.60 -20 0 -4 -1.50 6.60 20 0 4 -1.20 6.80 -20 0 -4 10.10 6.10 -20 -1 -4 18.40 9.70 20 -1 4 23.40 7.60 -20 1 4 3.60 6.30 -20 1 4 14.40 7.50 -20 1 4 6.70 3.10 -20 1 4 13.50 7.10 20 1 -4 14.80 7.80 -20 1 4 13.10 6.30 -20 -1 -4 7.30 7.00 -20 -1 -4 5.40 8.00 -20 -1 -4 12.70 5.50 -20 -1 4 13.00 8.00 -20 1 -4 10.30 6.90 -20 -1 4 5.70 6.20 -20 -1 4 8.50 3.40 -20 1 -4 -0.40 3.80 -20 1 -4 3.40 6.90 -20 1 -4 6.50 4.50 -20 -1 4 14.20 7.10 -20 -1 4 22.30 7.80 -20 1 -4 10.60 4.60 -20 1 -4 9.60 6.20 -20 -1 4 11.20 6.90 -21 0 0 -7.20 5.90 -21 0 0 -8.80 4.40 -21 0 0 14.30 8.30 -21 0 0 4.70 4.50 -21 0 0 8.60 6.30 -21 0 0 0.30 5.20 -21 0 0 -14.10 5.30 -21 0 0 -6.10 4.40 -21 1 0 -1.00 4.50 -21 -1 0 -2.80 6.30 -21 1 0 5.60 6.60 -21 -1 0 2.10 6.20 -21 1 0 1.00 6.10 -21 -1 0 3.60 4.30 -21 1 0 -11.40 3.60 -21 1 0 -3.90 5.00 -21 1 0 3.10 4.60 -21 1 0 8.10 6.30 -21 -1 0 14.00 6.60 -21 1 0 -8.40 5.40 -21 -1 0 -13.70 6.00 -21 -1 0 4.00 5.30 -21 0 -1 41.90 8.60 -21 0 1 28.20 6.70 -21 0 1 36.60 7.50 -21 0 -1 50.59 10.10 -21 0 -1 24.60 5.20 -21 0 1 35.50 6.40 -21 0 1 37.30 7.90 -21 0 1 41.60 9.60 -21 0 1 24.50 13.70 -21 0 -1 31.50 8.50 -21 0 -1 31.80 7.10 -21 0 1 39.90 9.00 -21 0 -1 33.20 7.80 -21 0 1 35.30 7.80 -21 1 1 11.40 5.00 -21 1 1 38.00 9.50 -21 -1 -1 17.70 8.10 -21 1 1 30.50 9.70 -21 1 1 9.10 12.00 -21 1 1 14.90 5.10 -21 1 1 7.70 5.60 -21 1 1 19.20 6.30 -21 -1 -1 25.50 6.90 -21 -1 -1 20.60 7.30 -21 -1 -1 23.10 7.00 -21 -1 -1 20.20 4.90 -21 1 1 23.50 8.10 -21 1 -1 24.90 8.00 -21 1 -1 47.50 9.50 -21 1 -1 20.30 6.90 -21 -1 1 18.60 8.20 -21 1 -1 15.40 6.30 -21 -1 1 18.50 8.00 -21 -1 1 25.30 7.40 -21 1 -1 12.80 5.10 -21 -1 1 10.20 7.60 -21 1 -1 6.70 6.40 -21 -1 1 21.10 5.60 -21 1 -1 18.50 5.60 -21 0 2 38.50 7.50 -21 0 -2 30.60 8.10 -21 0 -2 27.00 6.80 -21 0 2 36.50 9.30 -21 0 -2 32.90 5.40 -21 0 2 24.80 5.50 -21 0 -2 35.40 11.20 -21 0 -2 30.90 9.50 -21 0 2 27.30 8.00 -21 0 -2 25.90 7.60 -21 0 2 36.30 7.30 -21 -1 -2 17.80 4.40 -21 1 2 17.50 8.00 -21 -1 -2 5.50 3.30 -21 -1 -2 33.20 7.60 -21 1 2 13.70 5.30 -21 -1 -2 23.90 7.60 -21 -1 -2 10.90 7.10 -21 1 2 18.20 6.80 -21 1 2 11.90 5.00 -21 -1 -2 22.80 7.40 -21 -1 2 17.90 6.90 -21 1 -2 7.80 7.60 -21 -1 2 14.20 8.00 -21 1 -2 19.40 7.80 -21 1 -2 30.50 8.80 -21 1 -2 17.60 6.70 -21 1 -2 21.10 6.10 -21 -1 2 11.00 6.40 -21 -1 2 15.30 5.20 -21 1 -2 16.80 5.40 -21 -1 2 9.90 7.50 -21 1 -2 11.10 6.80 -21 -1 2 14.10 5.90 -21 1 -2 9.20 4.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 8611 _shelx_res_file ; TITL UMD2221G_a.res in Pnma umd2221g_a.res created by SHELXL-2018/3 at 09:22:23 on 04-Jun-2023 REM Old TITL UMD2221G in Pnma REM SHELXT solution in Pnma REM R1 0.074, Rweak 0.004, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C7 N Ni O9 S CELL 0.71073 17.1196 7.0609 11.2233 90 90 90 ZERR 4 0.0008 0.0003 0.0005 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Ni N O S UNIT 28 76 4 4 36 4 EQIV $1 0.5-X,0.5+Y,0.5+Z EQIV $2 +X,1+Y,+Z EQIV $3 1-X,1-Y,-Z DFIX 0.78 0.01 O1 H1 O2 H2a O2 H2b O3 H3a O3 H3b DFIX 1.25 0.01 H2a H2b H3a H3b L.S. 10 PLAN 1 SIZE 0.03 0.04 0.17 TEMP 24 HTAB O1 O5_$2 HTAB O2 O6_$2 HTAB O2 O6_$3 HTAB O3 O4 HTAB O3 O5_$1 CONF BOND $H LIST 4 HTAB 2 fmap 2 acta MORE -1 OMIT 2 0 1 REM REM REM WGHT 0.030800 0.682100 FVAR 0.42419 NI1 3 0.390913 0.750000 0.198524 10.50000 0.02095 0.02450 = 0.01894 0.00000 -0.00045 0.00000 S1 6 0.333428 0.250000 -0.033969 10.50000 0.02130 0.02058 = 0.02293 0.00000 -0.00232 0.00000 O1 5 0.350072 0.750000 0.023457 10.50000 0.05642 0.02894 = 0.02999 0.00000 -0.01870 0.00000 O2 5 0.468776 0.962705 0.145365 11.00000 0.03015 0.03247 = 0.02995 0.00596 0.00158 -0.00176 O3 5 0.314059 0.540115 0.246011 11.00000 0.03481 0.03701 = 0.03434 -0.00780 0.01080 -0.01052 O4 5 0.298303 0.250000 0.084962 10.50000 0.05274 0.03864 = 0.03570 0.00000 0.01607 0.00000 O5 5 0.310293 0.079429 -0.098265 11.00000 0.05437 0.02689 = 0.04173 -0.00604 -0.02009 0.00080 O6 5 0.419760 0.250000 -0.017500 10.50000 0.02321 0.04346 = 0.05145 0.00000 0.00034 0.00000 N1 4 0.444656 0.750000 0.363354 10.50000 0.02426 0.02603 = 0.02205 0.00000 -0.00289 0.00000 C1 1 0.523080 0.750000 0.369165 10.50000 0.02522 0.03019 = 0.02771 0.00000 0.00079 0.00000 AFIX 43 H1A 2 0.551105 0.750000 0.298181 10.50000 -1.20000 AFIX 0 C2 1 0.564327 0.750000 0.475272 10.50000 0.02442 0.02730 = 0.02994 0.00000 -0.00444 0.00000 C3 1 0.521300 0.750000 0.579867 10.50000 0.03296 0.03395 = 0.02416 0.00000 -0.00859 0.00000 AFIX 43 H3 2 0.546992 0.750000 0.652878 10.50000 -1.20000 AFIX 0 C4 1 0.440328 0.750000 0.576756 10.50000 0.03231 0.02798 = 0.02430 0.00000 0.00037 0.00000 C5 1 0.404636 0.750000 0.465811 10.50000 0.02507 0.02706 = 0.02580 0.00000 -0.00223 0.00000 AFIX 43 H5 2 0.350357 0.750000 0.462450 10.50000 -1.20000 AFIX 0 C6 1 0.652429 0.750000 0.474816 10.50000 0.02192 0.05623 = 0.04442 0.00000 -0.00648 0.00000 PART -1 AFIX 137 H6A 2 0.671277 0.686857 0.544900 10.50000 -1.50000 H6B 2 0.671120 0.878180 0.474031 10.50000 -1.50000 H6C 2 0.670966 0.684963 0.405226 10.50000 -1.50000 AFIX 0 PART 0 C7 1 0.391886 0.750000 0.688638 10.50000 0.03925 0.06448 = 0.02508 0.00000 0.00117 0.00000 PART -1 AFIX 137 H7A 2 0.418880 0.818472 0.750001 10.50000 -1.50000 H7B 2 0.383346 0.621918 0.714204 10.50000 -1.50000 H7C 2 0.342529 0.809610 0.673085 10.50000 -1.50000 AFIX 0 PART 0 H1 2 0.335379 0.839616 -0.010755 11.00000 0.05659 H2A 2 0.454034 1.047665 0.106734 11.00000 0.04490 H2B 2 0.505624 0.923191 0.111540 11.00000 0.06237 H3A 2 0.277668 0.556964 0.285416 11.00000 0.04100 H3B 2 0.305024 0.459735 0.201244 11.00000 0.04817 HKLF 4 REM UMD2221G_a.res in Pnma REM wR2 = 0.0595, GooF = S = 1.102, Restrained GooF = 1.100 for all data REM R1 = 0.0228 for 1386 Fo > 4sig(Fo) and 0.0262 for all 1499 data REM 128 parameters refined using 7 restraints END WGHT 0.0308 0.6819 REM Instructions for potential hydrogen bonds HTAB O1 S1_$2 HTAB O1 O5_$2 HTAB O2 S1_$2 HTAB O2 O6_$2 HTAB O2 O6_$3 HTAB O3 O5_$1 HTAB O3 O4 REM Highest difference peak 0.436, deepest hole -0.334, 1-sigma level 0.052 Q1 1 0.3499 0.2500 0.1014 10.50000 0.05 0.44 ; _shelx_res_checksum 77543 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -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 0.39091(2) 0.750000 0.19852(3) 0.02146(11) Uani d 1 . . S S1 0.33343(3) 0.250000 -0.03397(5) 0.02160(14) Uani d 1 . . O O1 0.35007(14) 0.750000 0.02346(18) 0.0384(5) Uani d 1 . . O O2 0.46878(7) 0.9627(2) 0.14536(12) 0.0309(3) Uani d 1 . . O O3 0.31406(8) 0.5401(2) 0.24601(12) 0.0354(3) Uani d 1 . . O O4 0.29830(12) 0.250000 0.08496(18) 0.0424(5) Uani d 1 . . O O5 0.31029(8) 0.0794(2) -0.09827(12) 0.0410(3) Uani d 1 . . O O6 0.41976(10) 0.250000 -0.01750(19) 0.0394(5) Uani d 1 . . N N1 0.44466(12) 0.750000 0.36335(17) 0.0241(4) Uani d 1 . . C C1 0.52308(14) 0.750000 0.3692(2) 0.0277(5) Uani d 1 . . H H1A 0.551105 0.750000 0.298181 0.033 Uiso calc 1 . . C C2 0.56433(14) 0.750000 0.4753(2) 0.0272(5) Uani d 1 . . C C3 0.52130(15) 0.750000 0.5799(2) 0.0304(6) Uani d 1 . . H H3 0.546992 0.750000 0.652878 0.036 Uiso calc 1 . . C C4 0.44033(15) 0.750000 0.5768(2) 0.0282(5) Uani d 1 . . C C5 0.40464(14) 0.750000 0.4658(2) 0.0260(5) Uani d 1 . . H H5 0.350357 0.750000 0.462450 0.031 Uiso calc 1 . . C C6 0.65243(15) 0.750000 0.4748(3) 0.0409(7) Uani d 1 . . H H6A 0.671277 0.686857 0.544900 0.061 Uiso calc 0.5 A -1 H H6B 0.671120 0.878180 0.474031 0.061 Uiso calc 0.5 A -1 H H6C 0.670966 0.684963 0.405226 0.061 Uiso calc 0.5 A -1 C C7 0.39189(17) 0.750000 0.6886(2) 0.0429(7) Uani d 1 . . H H7A 0.418880 0.818472 0.750001 0.064 Uiso calc 0.5 B -1 H H7B 0.383346 0.621918 0.714204 0.064 Uiso calc 0.5 B -1 H H7C 0.342529 0.809610 0.673085 0.064 Uiso calc 0.5 B -1 H H1 0.3354(14) 0.840(3) -0.011(2) 0.057(8) Uiso d 1 . . H H2A 0.4540(12) 1.048(2) 0.1067(18) 0.045(7) Uiso d 1 . . H H2B 0.5056(10) 0.923(3) 0.1115(19) 0.062(9) Uiso d 1 . . H H3A 0.2777(9) 0.557(3) 0.2854(16) 0.041(6) Uiso d 1 . . H H3B 0.3050(12) 0.460(3) 0.2012(16) 0.048(7) Uiso d 1 . . 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 0.02095(16) 0.02450(18) 0.01894(17) 0.000 -0.00045(11) 0.000 S1 0.0213(3) 0.0206(3) 0.0229(3) 0.000 -0.0023(2) 0.000 O1 0.0564(13) 0.0289(11) 0.0300(10) 0.000 -0.0187(9) 0.000 O2 0.0301(7) 0.0325(7) 0.0300(7) -0.0018(6) 0.0016(5) 0.0060(6) O3 0.0348(7) 0.0370(8) 0.0343(7) -0.0105(6) 0.0108(6) -0.0078(7) O4 0.0527(12) 0.0386(12) 0.0357(11) 0.000 0.0161(9) 0.000 O5 0.0544(8) 0.0269(7) 0.0417(8) 0.0008(6) -0.0201(6) -0.0060(6) O6 0.0232(9) 0.0435(12) 0.0515(12) 0.000 0.0003(8) 0.000 N1 0.0243(9) 0.0260(11) 0.0221(10) 0.000 -0.0029(8) 0.000 C1 0.0252(11) 0.0302(14) 0.0277(13) 0.000 0.0008(10) 0.000 C2 0.0244(12) 0.0273(13) 0.0299(13) 0.000 -0.0044(10) 0.000 C3 0.0330(13) 0.0339(14) 0.0242(12) 0.000 -0.0086(10) 0.000 C4 0.0323(12) 0.0280(13) 0.0243(12) 0.000 0.0004(10) 0.000 C5 0.0251(11) 0.0271(13) 0.0258(12) 0.000 -0.0022(9) 0.000 C6 0.0219(12) 0.0562(19) 0.0444(17) 0.000 -0.0065(11) 0.000 C7 0.0392(15) 0.064(2) 0.0251(14) 0.000 0.0012(11) 0.000 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 O1 Ni1 O2 . 7_575 86.85(6) ? O1 Ni1 O2 . . 86.85(6) ? O2 Ni1 O2 7_575 . 91.60(8) ? O3 Ni1 O1 7_575 . 91.70(6) ? O3 Ni1 O1 . . 91.70(6) ? O3 Ni1 O2 7_575 . 87.95(6) ? O3 Ni1 O2 . . 178.51(6) ? O3 Ni1 O2 . 7_575 87.95(6) ? O3 Ni1 O2 7_575 7_575 178.51(6) ? O3 Ni1 O3 . 7_575 92.46(8) ? O3 Ni1 N1 7_575 . 93.04(6) ? O3 Ni1 N1 . . 93.04(6) ? N1 Ni1 O1 . . 173.14(9) ? N1 Ni1 O2 . . 88.38(5) ? N1 Ni1 O2 . 7_575 88.37(5) ? O4 S1 O6 . . 107.12(13) ? O5 S1 O4 7_565 . 109.84(8) ? O5 S1 O4 . . 109.85(8) ? O5 S1 O5 7_565 . 111.30(11) ? O5 S1 O6 . . 109.32(8) ? O5 S1 O6 7_565 . 109.32(8) ? Ni1 O1 H1 . . 124.8(19) ? Ni1 O1 H1 . 7_575 124.8(19) ? H1 O1 H1 . 7_575 108(4) ? Ni1 O2 H2A . . 120.2(17) ? Ni1 O2 H2B . . 113.1(19) ? H2A O2 H2B . . 105.3(15) ? Ni1 O3 H3A . . 123.6(16) ? Ni1 O3 H3B . . 119.3(16) ? H3A O3 H3B . . 108.9(15) ? C1 N1 Ni1 . . 119.23(17) ? C5 N1 Ni1 . . 122.77(16) ? C5 N1 C1 . . 118.0(2) ? N1 C1 H1A . . 118.3 ? N1 C1 C2 . . 123.4(2) ? C2 C1 H1A . . 118.3 ? C1 C2 C3 . . 117.2(2) ? C1 C2 C6 . . 120.5(2) ? C3 C2 C6 . . 122.3(2) ? C2 C3 H3 . . 119.7 ? C2 C3 C4 . . 120.7(2) ? C4 C3 H3 . . 119.7 ? C3 C4 C5 . . 117.6(2) ? C3 C4 C7 . . 122.0(2) ? C5 C4 C7 . . 120.4(2) ? N1 C5 C4 . . 123.1(2) ? N1 C5 H5 . . 118.5 ? C4 C5 H5 . . 118.5 ? C2 C6 H6A . . 109.5 ? C2 C6 H6B . . 109.5 ? C2 C6 H6C . . 109.5 ? H6A C6 H6B . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? C4 C7 H7A . . 109.5 ? C4 C7 H7B . . 109.5 ? C4 C7 H7C . . 109.5 ? H7A C7 H7B . . 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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 O1 . 2.0855(19) ? Ni1 O2 . 2.0949(13) ? Ni1 O2 7_575 2.0949(13) ? Ni1 O3 . 2.0522(13) ? Ni1 O3 7_575 2.0522(13) ? Ni1 N1 . 2.066(2) ? S1 O4 . 1.464(2) ? S1 O5 7_565 1.4588(14) ? S1 O5 . 1.4588(14) ? S1 O6 . 1.4895(19) ? O1 H1 7_575 0.782(10) ? O1 H1 . 0.782(10) ? O2 H2A . 0.782(9) ? O2 H2B . 0.787(9) ? O3 H3A . 0.773(9) ? O3 H3B . 0.774(9) ? N1 C1 . 1.344(3) ? N1 C5 . 1.339(3) ? C1 H1A . 0.9300 ? C1 C2 . 1.384(3) ? C2 C3 . 1.386(4) ? C2 C6 . 1.508(3) ? C3 H3 . 0.9300 ? C3 C4 . 1.387(4) ? C4 C5 . 1.387(3) ? C4 C7 . 1.505(4) ? C5 H5 . 0.9300 ? C6 H6A . 0.9600 ? C6 H6B . 0.9600 ? C6 H6C . 0.9600 ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? 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 _geom_hbond_publ_flag O1 H1 O5 1_565 0.782(10) 2.004(10) 2.7822(18) 174(3) yes O2 H2A O6 1_565 0.782(9) 2.081(10) 2.857(2) 172(2) yes O2 H2B O6 5_665 0.787(9) 2.059(12) 2.821(2) 163(3) yes O3 H3A O5 8_666 0.773(9) 1.999(10) 2.7683(18) 173(2) yes O3 H3B O4 . 0.774(9) 1.977(9) 2.745(2) 172(2) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ni1 N1 C1 C2 . . . . 180.000000 ? Ni1 N1 C5 C4 . . . . 180.000000 ? N1 C1 C2 C3 . . . . 0.000000 ? N1 C1 C2 C6 . . . . 180.000000 ? C1 N1 C5 C4 . . . . 0.000000 ? C1 C2 C3 C4 . . . . 0.000000 ? C2 C3 C4 C5 . . . . 0.000000 ? C2 C3 C4 C7 . . . . 180.000000 ? C3 C4 C5 N1 . . . . 0.000000 ? C5 N1 C1 C2 . . . . 0.000000 ? C6 C2 C3 C4 . . . . 180.000000 ? C7 C4 C5 N1 . . . . 180.000000 ? _cod_database_fobs_code 2022796