#------------------------------------------------------------------------------ #$Date: 2019-01-16 05:22:18 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213107 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242809.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_2242809 loop_ _publ_author_name 'Jochriem, Markus' 'Wurst, Klaus' 'Kopacka, Holger' 'Bildstein, Benno' _publ_section_title ; Crystal structures of 1'-aminocobaltocenium-1-carboxylic acid chloride monohydrate and of its azo dye 1'-[2-(1-amino-2,6-dimethylphenyl)diazen-1-yl]cobaltocenium-1-carboxylic acid hexafluoridophosphate monohydrate ; _journal_coeditor_code WM5478 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 208 _journal_page_last 213 _journal_paper_doi 10.1107/S2056989019000562 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '[Co (C5 H6 N) (C6 H5 O2)] Cl, H2 O' _chemical_formula_moiety 'C11 H11 Co N O2 +, Cl -, H2 O' _chemical_formula_sum 'C11 H13 Cl Co N O3' _chemical_formula_weight 301.60 _chemical_name_systematic ; 1'-Aminocobaltocenium-1-carboxylic acid chloride monohydrate ; _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.7269(5) _cell_length_b 6.7024(3) _cell_length_c 11.7607(4) _cell_measurement_reflns_used 9295 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 50.7 _cell_measurement_theta_min 2.7 _cell_volume 1160.85(8) _computing_cell_refinement ; SAINT (Bruker, 2013) ; _computing_data_collection ; APEX3 (Bruker, 2013) ; _computing_data_reduction ; SAINT (Bruker, 2013) ; _computing_molecular_graphics ; CHEMDRAW (Cambridge Soft, 2001) and ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 193(2) _diffrn_detector_area_resol_mean 10.4 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multi layered optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_unetI/netI 0.0220 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14289 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.715 _diffrn_reflns_theta_min 2.766 _diffrn_source 'Incoatec Microfocus' _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.726 _exptl_crystal_description plate _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.495 _refine_diff_density_min -0.312 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.067(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 2163 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0195 _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^)+(0.0262P)^2^+0.1150P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0459 _reflns_number_gt 2099 _reflns_number_total 2163 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5478sup1.cif _cod_data_source_block 3 _cod_database_code 2242809 _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 0.809 _shelx_estimated_absorpt_t_max 0.951 _shelx_hkl_file ; 0 -1 0 1189.88 40.30 0 1 0 1240.48 40.40 0 -2 0 324.37 11.70 0 2 0 317.17 11.90 0 2 0 340.27 11.90 0 3 0 26.50 2.70 0 -3 0 23.00 2.30 0 3 0 25.10 2.70 0 -4 0 8163.78 268.77 0 4 0 8107.29 266.47 0 4 0 7904.21 266.67 0 5 0 1229.08 43.60 0 -5 0 1292.17 44.80 0 5 0 1220.98 43.90 0 -5 0 1221.68 43.10 0 6 0 28.10 5.10 0 -6 0 22.60 5.20 0 6 0 33.90 5.10 0 -6 0 24.10 3.70 0 -7 0 79.09 11.60 0 -7 0 73.59 6.90 0 7 0 70.59 9.80 0 7 0 75.29 9.60 0 8 0 468.35 23.30 0 8 0 464.65 22.10 0 -8 0 428.66 25.10 0 -8 0 437.36 19.10 0 -1 1 1.50 0.70 0 1 -1 1.40 0.60 0 -1 -1 1.50 0.60 0 1 -1 1.20 0.70 0 -1 1 1.10 0.50 0 1 1 1.10 0.40 0 1 1 1.00 0.60 0 -1 -1 1.20 0.50 0 -1 1 1.80 0.70 0 -2 -1 0.70 0.70 0 -2 -1 -0.10 0.80 0 -2 1 0.50 0.90 0 2 1 1.00 0.90 0 -2 1 0.40 1.00 0 2 -1 0.40 0.90 0 2 1 -0.70 0.70 0 3 -1 0.20 1.20 0 -3 1 1.60 1.50 0 -3 1 0.10 1.10 0 3 1 0.70 1.30 0 -3 -1 0.40 0.90 0 3 1 0.00 1.10 0 4 1 -0.70 1.80 0 -4 -1 -1.50 1.50 0 4 1 -0.60 1.80 0 4 -1 0.60 2.10 0 -4 1 -1.30 1.60 0 4 -1 -1.10 1.80 0 -4 1 -0.40 2.00 0 5 1 1.30 2.80 0 5 -1 -2.20 2.60 0 -5 -1 -0.60 1.70 0 -5 1 2.60 3.20 0 5 -1 -3.00 2.50 0 -5 1 1.80 2.10 0 5 1 3.10 2.60 0 -6 1 -1.90 2.60 0 6 1 1.10 3.40 0 6 1 -1.60 3.50 0 6 -1 0.00 3.60 0 6 -1 1.40 3.90 0 -6 -1 0.00 4.20 0 -6 -1 -1.80 2.10 0 -6 1 -0.10 3.90 0 -7 -1 -0.70 3.30 0 7 1 2.40 4.90 0 -7 1 -1.70 3.30 0 -7 1 -1.40 5.30 0 -7 -1 2.40 6.10 0 7 -1 -2.10 4.60 0 7 -1 -1.60 5.10 0 7 1 1.20 5.40 0 8 1 -1.70 6.90 0 -8 1 9.40 8.80 0 8 -1 2.60 7.60 0 -8 1 6.40 4.40 0 -8 -1 2.30 4.30 0 8 1 -0.20 7.20 0 8 -1 4.40 7.60 0 -8 1 1.20 3.30 0 -8 -1 -6.90 9.50 0 0 -2 7220.78 230.78 0 0 2 6663.83 230.88 0 0 -2 6815.62 230.98 0 0 -2 7122.29 231.28 0 0 2 6988.40 231.08 0 1 -2 741.43 26.00 0 -1 -2 781.12 26.00 0 1 2 779.12 26.00 0 1 -2 782.52 26.30 0 -1 2 780.32 26.00 0 1 -2 772.92 26.00 0 -1 2 760.72 26.00 0 2 2 697.33 24.00 0 -2 2 713.83 24.30 0 -2 -2 697.43 23.90 0 2 -2 736.53 24.90 0 -2 2 719.73 24.70 0 2 2 708.53 24.50 0 -2 2 699.53 24.60 0 -2 -2 710.63 24.40 0 -3 2 125.29 5.40 0 3 2 117.79 5.70 0 -3 -2 108.29 4.90 0 -3 -2 110.89 5.50 0 -3 2 121.89 5.80 0 3 -2 111.49 6.00 0 3 2 120.69 5.20 0 -3 2 118.89 6.00 0 4 2 3690.13 126.89 0 -4 -2 3856.21 126.69 0 -4 2 3745.73 127.49 0 4 -2 3952.80 127.99 0 -4 2 3871.01 128.09 0 4 2 3785.22 127.49 0 5 2 397.36 16.30 0 5 -2 382.66 16.40 0 -5 -2 370.16 14.90 0 5 -2 386.76 16.60 0 -5 2 431.56 16.10 0 5 2 403.66 15.70 0 -5 2 399.56 17.00 0 6 -2 38.00 5.50 0 -6 2 35.30 5.50 0 6 2 32.40 4.90 0 6 2 29.60 5.10 0 -6 2 26.70 5.50 0 6 -2 51.49 7.10 0 -6 -2 46.90 4.40 0 -6 2 32.50 4.50 0 -7 -2 18.50 3.70 0 -7 -2 14.60 6.40 0 7 2 20.30 6.20 0 7 -2 28.20 6.80 0 -7 2 18.40 3.60 0 -7 2 22.20 4.70 0 7 2 22.60 5.70 0 7 -2 27.70 6.30 0 -7 2 24.50 6.80 0 8 2 555.34 25.10 0 -8 2 590.64 23.60 0 -8 2 510.45 22.40 0 -8 -2 599.14 22.10 0 8 -2 552.94 26.50 0 8 -2 579.14 26.10 0 8 2 525.15 25.50 0 -8 2 539.95 27.70 0 0 -3 0.50 0.60 0 0 -3 0.10 0.60 0 0 -3 0.60 0.50 0 0 3 0.20 0.60 0 0 -3 0.20 0.60 0 1 -3 1.50 0.90 0 1 -3 1.10 0.60 0 -1 -3 1.20 0.70 0 -1 3 1.30 0.80 0 1 -3 2.60 0.80 0 -1 3 1.80 0.70 0 1 3 1.40 0.80 0 -1 3 1.30 0.90 0 2 -3 -0.30 0.90 0 2 -3 0.40 1.30 0 2 3 0.50 1.00 0 -2 3 1.40 0.80 0 -2 3 -1.20 1.10 0 -2 3 -1.20 1.00 0 -2 -3 0.80 0.90 0 -2 -3 0.00 0.60 0 -3 3 0.50 1.40 0 3 -3 2.00 1.60 0 3 3 1.40 1.10 0 -3 3 0.50 1.50 0 3 3 0.90 1.40 0 -3 -3 -0.30 0.80 0 -3 -3 1.20 1.20 0 -3 3 2.30 1.10 0 4 3 1.50 2.10 0 4 3 0.50 1.60 0 4 -3 1.80 2.20 0 -4 3 -0.90 1.20 0 -4 3 -0.50 1.80 0 -4 -3 0.20 1.20 0 -4 3 -1.00 2.10 0 -5 3 -3.40 2.30 0 -5 3 0.20 1.80 0 5 3 -0.20 2.40 0 -5 3 -1.10 3.10 0 -5 -3 2.90 1.50 0 5 -3 2.40 3.00 0 5 3 1.10 2.40 0 -6 3 -3.40 4.40 0 -6 3 -0.40 2.20 0 6 -3 0.30 4.20 0 -6 3 0.10 2.90 0 6 3 0.80 4.00 0 6 3 1.70 3.50 0 -6 -3 -0.50 1.80 0 6 -3 -3.50 3.90 0 7 3 2.90 5.00 0 -7 3 1.40 4.00 0 7 3 5.70 5.10 0 7 -3 4.90 5.80 0 -7 -3 -1.60 2.90 0 7 -3 1.60 5.70 0 -7 -3 -8.60 5.60 0 -7 3 -1.70 3.10 0 -7 3 -1.30 6.10 0 -8 3 3.40 4.00 0 -8 3 -1.10 9.10 0 0 -4 6457.35 212.78 0 0 -4 6212.38 213.68 0 0 -4 6408.76 212.88 0 0 -4 6565.24 213.18 0 1 4 1254.07 42.90 0 1 -4 1322.47 43.00 0 1 -4 1224.38 43.00 0 -1 4 1242.68 43.30 0 -1 -4 1293.57 42.60 0 -1 4 1245.28 42.90 0 1 -4 1350.86 43.50 0 -1 -4 1300.57 43.10 0 2 -4 815.42 27.60 0 -2 4 767.82 27.40 0 -2 -4 790.92 26.80 0 2 -4 833.62 28.20 0 2 4 769.92 27.30 0 -2 4 793.52 27.90 0 -2 4 787.12 27.50 0 2 -4 774.72 27.50 0 -2 -4 824.32 27.50 0 3 -4 242.18 9.60 0 -3 -4 225.98 8.30 0 -3 4 223.08 9.70 0 3 4 220.18 9.30 0 3 -4 225.58 9.90 0 -3 -4 234.68 9.30 0 -3 4 218.48 9.50 0 -3 4 232.08 9.30 0 -4 4 919.31 33.30 0 -4 4 916.11 33.30 0 4 4 893.41 32.80 0 -4 4 905.21 32.60 0 4 -4 975.60 34.00 0 -4 -4 958.40 32.80 0 -4 -4 938.31 31.60 0 -5 -4 721.93 25.10 0 5 4 692.83 26.70 0 -5 4 722.53 27.20 0 -5 4 719.93 26.30 0 -5 4 714.53 27.40 0 5 -4 747.43 28.10 0 6 -4 289.17 14.70 0 -6 -4 285.47 11.40 0 -6 4 304.47 15.30 0 -6 4 302.37 13.80 0 -6 4 286.37 12.90 0 6 4 283.47 14.20 0 -7 4 52.09 8.50 0 -7 -4 43.20 4.50 0 -7 4 46.60 6.00 0 7 4 46.50 7.20 0 7 -4 40.40 7.40 0 -7 4 55.59 6.40 0 7 -4 41.10 7.50 0 0 -5 4.10 1.00 0 0 -5 3.40 1.00 0 0 -5 3.80 1.00 0 0 -5 2.60 1.00 0 1 -5 1.00 1.20 0 -1 -5 0.30 0.70 0 -1 5 1.50 1.00 0 -1 5 0.40 1.10 0 -1 -5 3.40 1.00 0 1 -5 1.50 0.90 0 -2 -5 3.20 1.10 0 2 -5 1.90 1.50 0 -2 5 -0.10 1.40 0 2 -5 2.50 1.10 0 -2 5 2.90 1.60 0 -3 -5 4.10 1.50 0 -3 5 2.20 1.80 0 -3 5 2.60 1.90 0 3 5 5.80 1.80 0 3 -5 3.90 1.60 0 3 -5 1.20 1.80 0 -4 5 0.40 2.50 0 4 5 0.00 1.90 0 -4 5 2.20 2.20 0 -4 -5 -0.30 1.70 0 -4 -5 -0.90 0.90 0 -4 5 -0.20 1.50 0 4 -5 -0.50 2.40 0 -5 -5 0.20 1.30 0 5 5 2.80 3.00 0 -5 5 2.90 3.30 0 5 -5 5.80 3.10 0 -5 5 2.10 3.00 0 -5 5 2.70 2.00 0 6 -5 -7.90 3.80 0 -6 -5 0.30 1.60 0 6 5 2.90 4.10 0 -6 5 -0.60 2.80 0 -6 5 0.70 4.70 0 -6 5 -0.20 3.50 0 -7 -5 0.60 2.20 0 7 5 0.50 6.00 0 -7 5 3.70 3.20 0 -7 5 -4.20 4.40 0 7 -5 3.70 5.90 0 -7 5 -1.60 6.70 0 7 -5 -7.20 5.80 0 0 -6 344.97 12.60 0 0 -6 322.67 12.60 0 0 -6 349.47 12.70 0 0 -6 334.67 12.40 0 1 -6 266.57 11.10 0 -1 6 311.27 11.20 0 1 -6 258.97 10.70 0 1 -6 257.37 10.50 0 -1 -6 271.97 10.60 0 -1 -6 276.67 10.30 0 -1 -6 274.07 10.70 0 -1 6 311.57 10.50 0 2 6 207.38 8.30 0 2 -6 194.98 9.20 0 -2 -6 199.18 8.30 0 -2 -6 197.78 7.40 0 -2 6 211.78 9.00 0 2 -6 181.68 8.50 0 -2 6 210.08 8.50 0 -2 6 207.08 8.30 0 2 -6 206.58 8.40 0 3 6 123.79 6.00 0 -3 6 134.89 6.90 0 -3 6 132.89 6.30 0 -3 -6 101.39 4.70 0 -3 -6 93.29 5.80 0 3 -6 108.19 6.70 0 3 -6 109.49 6.00 0 -3 6 137.99 6.40 0 -4 -6 633.14 22.10 0 4 -6 614.54 23.40 0 4 6 568.04 21.80 0 -4 6 577.24 22.30 0 -4 6 543.75 22.60 0 -4 6 583.54 22.30 0 -4 -6 626.14 20.20 0 5 -6 142.09 9.60 0 -5 -6 139.79 5.90 0 -5 -6 146.79 8.20 0 -5 6 169.38 9.80 0 5 6 164.58 8.90 0 -5 6 156.98 8.40 0 -5 6 170.18 9.50 0 -6 6 175.58 12.10 0 6 -6 132.69 11.00 0 -6 6 172.08 9.30 0 6 6 181.88 10.70 0 -6 6 160.88 10.50 0 -6 -6 151.98 6.40 0 -7 6 -1.80 4.90 0 -7 6 -0.60 7.20 0 7 -6 1.70 6.50 0 -7 6 4.20 3.80 0 7 6 5.80 6.10 0 0 -7 2.00 1.20 0 0 -7 1.90 1.10 0 0 -7 1.40 1.30 0 0 -7 5.10 1.50 0 -1 -7 0.60 1.30 0 -1 7 0.80 1.30 0 1 -7 0.20 1.40 0 -1 -7 0.80 1.10 0 1 -7 1.00 1.30 0 1 -7 0.00 1.20 0 -1 -7 1.30 1.50 0 -1 7 1.20 1.50 0 -1 -7 2.10 1.20 0 -2 7 1.10 1.70 0 2 -7 -1.50 1.40 0 -2 7 0.00 1.40 0 -2 -7 1.40 1.00 0 2 -7 -1.60 1.70 0 -2 7 2.10 1.90 0 -2 -7 0.50 1.60 0 2 7 -0.30 1.50 0 -3 7 -0.80 2.50 0 3 -7 -1.40 2.20 0 -3 7 1.70 1.60 0 3 -7 -0.90 1.80 0 3 -7 3.80 2.10 0 -3 -7 0.80 1.20 0 3 7 1.90 2.00 0 -3 7 0.70 2.20 0 -3 -7 2.90 1.70 0 -3 -7 -0.40 0.70 0 -4 7 1.50 2.90 0 4 7 -0.50 2.20 0 -4 7 1.60 2.50 0 4 -7 -1.70 2.80 0 -4 -7 2.60 2.10 0 -4 7 -0.90 1.70 0 -5 7 3.30 3.80 0 -5 -7 -0.90 2.60 0 -5 7 -4.20 3.30 0 5 -7 -5.50 3.70 0 5 7 3.30 3.30 0 -5 7 -1.60 2.50 0 6 -7 -4.60 4.60 0 -6 7 -1.60 3.40 0 6 7 2.50 4.70 0 -6 7 -6.90 4.30 0 -6 7 -1.40 5.20 0 7 7 -4.50 6.20 0 7 -7 6.00 6.00 0 -7 7 3.80 7.70 0 -7 7 4.80 6.50 0 -7 7 -0.40 3.90 0 0 -8 2421.66 81.49 0 0 -8 2452.15 81.69 0 0 -8 2399.46 81.69 0 0 -8 2434.36 81.69 0 -1 -8 562.14 20.70 0 1 -8 557.24 20.40 0 1 -8 558.64 20.70 0 -1 -8 579.44 20.70 0 -1 8 570.94 20.80 0 -1 -8 556.44 20.20 0 1 -8 567.84 21.30 0 1 -8 564.14 20.80 0 -1 -8 567.04 20.60 0 -2 8 166.78 8.20 0 2 -8 174.58 8.90 0 2 -8 174.38 8.30 0 2 -8 179.38 7.90 0 -2 -8 177.08 8.00 0 -2 8 172.08 8.70 0 2 8 174.58 7.70 0 -2 8 169.58 7.60 0 -2 -8 174.78 7.10 0 3 8 65.69 4.70 0 -3 8 64.89 4.70 0 -3 8 63.19 4.80 0 -3 -8 58.59 3.60 0 3 -8 53.69 5.20 0 -3 -8 60.09 4.70 0 -3 -8 56.89 3.10 0 3 -8 50.49 5.60 0 3 -8 51.79 4.60 0 -3 8 74.09 6.20 0 -4 -8 434.96 16.00 0 -4 8 362.56 15.70 0 -4 8 394.66 17.10 0 -4 8 373.76 15.80 0 4 8 367.36 15.40 0 4 -8 421.96 17.60 0 -5 8 617.34 25.20 0 -5 8 619.34 24.20 0 5 8 623.84 23.90 0 -5 -8 640.14 24.00 0 5 -8 609.24 25.90 0 -5 8 635.74 24.60 0 6 8 147.59 10.70 0 6 -8 122.59 11.20 0 -6 8 135.79 9.20 0 -6 8 140.69 11.20 0 -6 8 147.89 12.10 0 0 -9 1.00 1.80 0 0 -9 1.10 1.70 0 0 -9 0.60 1.70 0 0 -9 2.60 2.00 0 -1 -9 0.40 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2 6 7 32.70 5.30 -2 6 -7 42.20 6.60 -2 -6 7 40.40 5.70 -2 -6 7 24.10 5.50 2 -6 -7 36.80 5.30 -2 -7 -7 15.30 2.70 -2 7 7 17.40 7.60 2 -7 7 27.80 8.70 -2 7 -7 16.20 6.50 2 7 7 19.80 6.80 -2 -7 7 8.60 4.10 -2 -7 7 21.60 8.50 -2 0 -8 296.87 11.80 -2 0 -8 289.17 11.50 -2 0 -8 282.17 11.30 2 0 -8 271.87 10.90 2 0 -8 293.57 12.00 2 0 -8 277.77 11.70 -2 0 8 333.27 11.70 -2 0 -8 292.37 12.00 2 0 -8 276.37 11.80 2 -1 8 345.77 12.80 2 1 -8 313.37 11.70 -2 -1 -8 322.47 13.00 -2 -1 -8 305.77 12.20 2 1 -8 310.47 13.20 2 1 -8 320.37 12.90 -2 -1 -8 313.47 12.30 2 -1 8 318.07 12.60 2 1 -8 312.77 12.90 -2 -1 -8 308.47 12.00 2 -1 -8 313.47 12.10 -2 -1 8 328.77 12.90 -2 1 -8 316.87 12.50 -2 1 -8 309.57 13.10 2 -1 -8 319.17 12.70 -2 1 -8 304.47 12.90 2 -1 -8 310.57 13.00 2 2 -8 143.69 8.10 2 -2 8 143.49 7.20 2 2 -8 128.69 5.90 -2 2 8 136.49 7.20 2 2 -8 121.59 8.10 -2 -2 -8 134.19 7.20 -2 -2 -8 133.29 6.20 2 -2 8 138.69 7.00 -2 -2 -8 138.89 6.50 2 -2 -8 131.19 5.60 2 -2 -8 136.29 7.20 -2 2 -8 133.79 7.30 -2 2 -8 146.29 7.20 -2 2 -8 142.89 7.80 -2 -2 8 137.89 7.70 -2 -2 8 137.69 7.00 2 3 -8 69.69 6.40 -2 3 8 68.89 5.70 2 -3 8 75.29 5.50 -2 -3 -8 66.49 4.50 2 3 -8 67.59 5.70 2 -3 8 71.59 5.90 -2 3 -8 73.79 5.90 2 -3 -8 59.49 5.50 -2 3 -8 70.39 5.60 -2 -3 8 67.49 4.90 2 3 8 75.49 4.20 -2 -3 8 71.59 6.60 -2 -3 8 73.59 4.30 2 -4 8 224.18 11.40 -2 -4 -8 233.98 9.60 2 -4 8 222.28 10.50 -2 -4 -8 232.18 9.90 -2 4 8 228.28 11.00 2 4 -8 230.08 12.30 -2 4 -8 240.48 11.40 -2 -4 8 212.98 10.60 -2 -4 8 242.68 12.20 -2 -4 8 219.18 9.90 2 -4 -8 227.68 11.10 2 4 8 228.18 9.70 -2 4 -8 211.28 11.30 -2 5 8 232.78 12.10 2 5 -8 208.08 12.60 -2 -5 -8 215.28 9.10 2 -5 8 225.98 11.10 2 -5 8 249.38 13.00 2 5 8 222.88 10.30 -2 -5 8 245.08 13.00 -2 -5 8 221.08 11.20 2 -5 -8 200.48 11.40 -2 5 -8 219.88 12.80 -2 -5 8 221.98 11.40 2 -6 8 101.79 11.90 2 -6 8 94.69 8.30 -2 -6 -8 103.79 5.40 -2 6 8 127.49 11.20 2 6 -8 115.09 10.80 -2 -6 8 107.69 11.00 -2 -6 8 126.29 8.30 2 -6 -8 99.09 9.00 -2 6 -8 102.89 10.50 2 6 8 116.49 9.20 -2 -6 8 120.39 11.30 -2 0 -9 39.30 4.00 2 0 -9 44.50 4.10 -2 0 -9 44.70 4.40 2 0 -9 43.10 3.40 2 0 -9 45.60 6.10 -2 0 -9 39.80 3.60 2 0 -9 39.20 4.30 -2 0 -9 37.50 4.00 -2 -1 -9 48.40 3.90 -2 -1 -9 42.30 4.20 -2 -1 -9 45.10 4.00 2 -1 9 50.79 4.70 2 1 -9 43.00 4.50 2 1 -9 44.60 3.40 -2 -1 -9 46.80 3.80 2 1 -9 50.49 5.00 2 1 -9 42.00 4.50 -2 -1 9 52.09 4.80 2 -1 -9 50.69 4.50 -2 1 -9 40.00 4.70 2 -1 -9 49.20 4.90 2 -1 -9 39.50 3.50 -2 1 -9 39.10 4.40 2 -1 -9 45.40 3.70 -2 1 -9 43.30 4.30 2 2 -9 -0.70 2.40 2 2 -9 2.70 3.30 -2 2 9 2.80 2.00 2 2 -9 0.20 2.40 -2 -2 -9 2.20 1.70 -2 -2 -9 1.80 2.20 2 -2 9 0.70 2.00 -2 -2 -9 3.60 2.00 2 -2 9 0.40 2.30 2 2 -9 3.10 1.70 -2 -2 -9 3.20 1.60 2 -2 -9 3.40 1.60 2 -2 -9 4.20 2.50 -2 2 -9 0.50 2.80 -2 -2 9 2.70 2.00 -2 2 -9 6.10 2.60 -2 2 -9 5.40 2.60 -2 3 9 68.39 5.80 2 -3 9 65.39 5.60 -2 -3 -9 49.60 3.80 -2 -3 -9 59.49 4.40 2 -3 9 64.99 5.90 2 3 -9 62.19 6.00 2 3 -9 51.09 6.10 -2 -3 -9 60.69 4.80 -2 -3 9 64.89 6.50 -2 3 -9 62.99 5.80 -2 -3 9 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40.70 6.00 -10 0 -10 44.20 6.70 -10 0 10 56.99 7.80 -10 0 -10 40.30 3.40 10 0 -10 52.19 7.00 10 0 -10 40.30 6.60 10 -1 10 8.80 5.70 -10 -1 -10 9.70 4.60 10 1 -10 5.50 4.70 -10 1 10 11.10 4.10 10 1 -10 12.30 4.50 10 1 -10 17.30 5.60 10 -1 10 7.50 4.00 -10 1 -10 8.80 4.60 10 -1 -10 5.90 4.80 -10 1 -10 13.80 3.20 10 -1 -10 6.20 4.50 -10 -1 10 14.70 5.30 -10 2 10 4.30 5.50 10 -2 10 0.90 4.00 10 2 -10 12.70 5.70 -10 -2 -10 1.10 4.40 10 2 -10 2.60 4.20 10 2 -10 1.80 4.70 -10 2 10 1.00 3.20 10 -2 10 1.90 5.70 -10 2 -10 5.40 3.90 -10 -2 10 1.30 5.60 -10 2 -10 -0.40 4.80 10 -2 -10 8.20 4.70 10 -2 -10 -0.40 3.20 10 3 -10 53.29 7.50 10 -3 10 35.90 5.50 -10 -3 -10 42.10 7.60 10 -3 10 35.70 7.60 -10 -3 -10 68.49 8.50 -10 3 10 35.50 7.70 10 3 -10 55.79 7.90 10 3 -10 56.89 7.70 10 -3 -10 45.40 7.30 10 -3 -10 48.50 7.50 -10 3 -10 35.60 5.80 -10 3 -10 49.60 6.20 -10 -3 10 34.50 7.40 -10 3 -10 49.00 7.40 10 0 -11 270.97 15.60 10 0 -11 291.77 15.80 10 0 -11 334.77 16.20 -10 0 11 308.37 15.30 -10 0 -11 296.47 16.30 10 -1 11 219.88 11.80 -10 1 11 220.58 11.50 10 -1 11 229.98 14.70 10 1 -11 223.28 13.40 10 1 -11 219.08 13.80 10 1 -11 222.08 13.20 -10 -1 -11 220.38 13.90 -10 -1 11 222.08 14.00 10 -1 -11 197.68 13.50 -10 1 -11 212.88 10.20 10 -1 -11 201.78 13.40 -10 1 -11 204.18 13.80 -10 1 -11 213.08 12.80 -10 2 11 53.39 8.20 10 2 -11 42.40 7.60 -10 -2 -11 69.19 9.00 10 -2 11 53.69 8.70 10 2 -11 53.49 7.60 10 -2 11 38.00 5.80 -10 2 11 46.50 5.30 -10 2 -11 44.80 7.10 -10 2 -11 49.50 5.80 -10 2 -11 54.69 8.40 -10 -2 11 48.90 8.10 10 -2 -11 45.60 5.80 10 -2 -11 41.30 6.40 11 0 0 2.50 2.50 11 0 0 3.10 2.10 -11 0 0 0.20 2.60 -11 0 0 3.10 2.10 -11 0 0 1.20 3.00 -11 -1 0 109.09 8.70 -11 -1 0 100.19 6.90 -11 -1 0 107.29 5.70 11 -1 0 101.99 6.80 11 1 0 109.49 6.50 -11 1 0 104.39 6.40 -11 1 0 97.99 7.50 11 -1 0 111.79 7.10 11 1 0 102.29 6.10 -11 2 0 686.03 26.50 11 -2 0 672.53 25.90 -11 -2 0 682.03 25.30 -11 -2 0 644.24 26.80 11 2 0 684.83 24.50 11 -2 0 666.13 25.80 -11 2 0 668.73 25.50 11 -3 0 134.59 8.90 -11 -3 0 136.09 10.30 -11 -3 0 124.69 8.20 11 -3 0 136.59 9.20 -11 3 0 130.29 8.80 11 3 0 132.99 7.30 -11 3 0 125.99 9.40 11 4 0 11.60 3.30 -11 4 0 2.80 3.70 -11 -4 0 4.80 5.00 -11 -4 0 7.20 4.20 11 -4 0 9.20 3.90 11 -4 0 11.30 4.50 -11 4 0 5.60 4.20 -11 -5 0 60.99 7.40 -11 5 0 63.49 9.40 -11 5 0 65.59 9.50 11 -5 0 72.39 8.80 11 -5 0 67.89 8.90 -11 -5 0 71.39 10.40 11 5 0 67.89 7.10 -11 5 0 72.19 7.90 -11 6 0 146.99 14.30 -11 -6 0 135.39 11.00 11 -6 0 122.79 14.80 -11 -6 0 158.58 13.50 -11 6 0 146.49 11.40 11 6 0 147.19 10.20 -11 0 1 2.50 2.60 -11 0 -1 0.60 2.60 11 0 -1 2.80 1.90 -11 0 -1 -2.10 1.70 11 0 1 -1.00 2.30 -11 0 1 4.20 3.10 11 0 1 -0.10 2.10 -11 0 1 -2.30 2.00 11 0 -1 -0.90 2.60 -11 -1 -1 335.47 12.70 -11 1 1 323.27 14.80 11 1 -1 349.17 13.80 -11 1 1 327.97 13.90 -11 1 1 313.77 14.40 11 -1 1 327.07 14.30 11 -1 1 348.47 14.10 11 1 -1 321.87 13.20 -11 -1 -1 339.57 14.30 11 1 1 337.27 13.80 -11 1 -1 331.47 14.90 -11 -1 1 316.57 13.80 11 1 1 337.87 13.30 11 -1 -1 333.37 14.40 11 -1 -1 321.97 13.90 -11 -1 1 318.47 13.20 -11 -1 1 320.07 15.20 -11 1 -1 331.47 13.70 11 2 -1 31.80 4.70 -11 2 1 31.30 6.30 -11 -2 -1 38.50 5.30 11 -2 1 35.80 5.90 -11 -2 -1 35.50 5.40 11 -2 1 34.60 4.90 11 2 -1 30.40 2.90 -11 2 1 35.80 5.20 11 -2 -1 35.00 4.80 -11 2 -1 37.00 5.10 -11 -2 1 35.30 5.00 11 2 1 39.90 4.30 -11 -2 1 40.90 6.00 11 -2 -1 29.20 4.60 -11 3 1 340.17 15.80 11 -3 1 365.46 16.70 11 3 -1 358.56 13.00 11 3 -1 360.76 14.60 -11 -3 -1 358.96 15.30 -11 3 1 337.27 16.30 -11 -3 -1 364.86 17.40 11 -3 1 338.47 15.80 11 3 1 354.86 13.80 -11 -3 1 355.46 16.60 -11 3 -1 356.86 16.60 11 -3 -1 357.06 16.10 11 -3 -1 351.16 16.10 -11 -3 1 359.06 17.10 -11 3 -1 364.36 15.80 -11 4 1 65.19 8.30 -11 -4 -1 71.19 7.20 -11 4 1 63.09 8.10 11 -4 1 66.59 8.40 11 -4 1 78.49 7.80 -11 -4 -1 68.79 8.70 11 4 -1 71.19 6.30 -11 -4 1 72.69 6.60 11 -4 -1 70.89 8.10 11 4 1 69.89 5.60 11 -4 -1 74.99 8.30 -11 -4 1 64.79 9.60 -11 4 -1 74.99 8.50 -11 4 -1 77.69 7.60 -11 -5 -1 73.19 7.80 -11 5 1 76.69 9.80 11 5 -1 49.80 7.30 11 -5 1 56.69 8.00 -11 5 1 60.19 7.40 -11 -5 -1 78.29 10.60 11 -5 -1 68.29 8.30 -11 5 -1 47.00 7.40 -11 5 -1 60.99 7.70 11 -5 -1 78.79 9.10 -11 5 -1 67.39 9.80 -11 -5 1 56.79 7.40 -11 -5 1 79.09 10.30 11 5 1 74.69 6.70 11 6 -1 16.80 5.20 -11 -6 -1 22.50 7.80 -11 6 1 14.20 7.70 11 -6 1 26.80 9.10 -11 6 1 23.30 6.50 -11 -6 -1 11.70 5.20 -11 -6 1 21.10 5.40 11 -6 -1 -0.20 7.10 -11 6 -1 11.60 7.60 -11 6 -1 22.90 6.40 11 6 1 22.00 5.20 -11 -6 1 21.50 7.20 11 0 2 -1.70 2.20 -11 0 2 0.80 2.40 11 0 2 -0.60 2.30 -11 0 2 0.80 2.30 -11 0 -2 -1.00 1.60 -11 0 2 0.30 3.00 11 0 -2 0.90 2.60 -11 0 -2 2.80 3.00 11 0 -2 -1.20 1.70 -11 -1 -2 200.88 10.20 11 -1 2 188.48 9.40 -11 -1 -2 193.88 8.00 -11 -1 -2 205.48 11.50 11 1 -2 203.58 9.70 -11 1 2 195.38 9.70 11 1 -2 185.58 8.50 -11 1 2 178.18 9.90 11 -1 2 182.68 9.90 -11 1 2 187.88 10.30 11 1 2 207.88 8.70 11 -1 -2 196.68 9.40 -11 -1 2 194.28 11.20 -11 1 -2 191.58 9.10 11 1 2 189.98 9.70 11 -1 -2 200.48 10.30 -11 -1 2 184.68 9.20 -11 1 -2 190.98 10.70 -11 -1 2 186.58 9.00 11 2 -2 752.72 28.10 11 2 -2 726.23 26.70 11 -2 2 822.52 29.60 -11 2 2 778.92 28.80 -11 2 2 789.32 29.30 11 -2 2 798.22 28.70 -11 -2 -2 749.53 28.80 -11 -2 -2 750.22 30.20 -11 2 2 792.82 29.00 11 2 2 798.82 27.00 11 -2 -2 739.53 29.10 -11 -2 2 776.12 30.10 -11 2 -2 748.33 28.40 -11 -2 2 803.42 28.00 11 -2 -2 710.93 28.60 -11 2 -2 750.42 29.70 -11 3 2 359.16 17.30 -11 3 2 372.66 17.10 -11 -3 -2 383.86 18.40 11 3 -2 396.46 14.50 11 -3 2 399.46 17.00 11 3 -2 398.06 16.00 11 -3 2 367.86 17.60 -11 -3 -2 398.76 16.60 -11 3 -2 389.46 18.00 11 -3 -2 389.96 17.20 11 3 2 390.46 14.60 11 -3 -2 401.16 17.40 -11 -3 2 399.06 18.70 -11 -3 2 401.96 15.80 -11 3 -2 402.46 17.00 -11 4 2 82.49 8.50 11 4 -2 80.79 10.60 -11 -4 -2 85.79 9.20 11 -4 2 73.19 9.00 11 4 -2 84.79 8.80 -11 -4 -2 82.29 7.40 -11 4 -2 81.69 8.60 -11 4 -2 80.69 7.40 -11 -4 2 77.79 9.90 11 -4 -2 83.99 8.50 11 4 2 80.09 5.50 -11 4 -2 85.59 8.40 -11 -4 2 70.29 6.80 11 -4 -2 87.79 8.30 -11 -5 -2 3.60 4.20 11 5 -2 -0.60 5.30 11 5 -2 0.20 4.10 11 -5 2 -1.30 5.60 -11 5 2 3.70 4.00 -11 5 2 4.70 5.50 -11 -5 -2 5.20 5.60 11 5 2 4.50 3.30 -11 5 -2 -2.30 4.30 11 -5 -2 4.70 4.60 -11 -5 2 5.00 5.30 -11 5 -2 -7.30 4.50 -11 5 -2 3.20 4.50 -11 -5 2 1.70 5.20 11 -5 -2 -5.40 5.20 -11 -6 -2 115.39 10.10 11 6 -2 121.29 12.20 -11 6 2 130.49 10.60 -11 -6 -2 138.49 13.40 -11 6 2 125.79 15.70 11 -6 2 154.58 17.70 11 6 -2 100.49 9.70 11 6 2 132.99 8.90 11 6 2 128.69 9.90 -11 6 -2 117.79 11.40 11 -6 -2 118.59 14.40 -11 6 -2 98.49 13.80 -11 -6 2 125.89 14.00 11 -6 -2 96.29 10.80 -11 -6 2 116.49 10.30 11 0 -3 -3.30 2.60 -11 0 3 -0.30 2.30 -11 0 3 4.00 2.70 -11 0 -3 2.10 4.40 -11 0 -3 -0.40 1.50 -11 0 3 4.00 3.20 11 0 -3 -0.20 1.60 11 0 3 -1.90 2.30 11 1 -3 62.99 4.20 11 1 -3 53.69 5.80 -11 1 3 64.89 6.00 11 -1 3 56.19 6.10 -11 -1 -3 72.09 3.60 11 1 -3 73.89 4.70 11 -1 3 53.59 5.40 -11 1 3 56.89 6.20 -11 1 -3 66.59 5.00 -11 1 -3 69.89 6.60 -11 -1 3 57.09 5.30 -11 -1 3 54.99 5.40 11 -1 -3 68.39 5.20 11 1 3 62.39 4.50 -11 -1 3 54.69 6.80 -11 2 3 297.27 13.80 -11 -2 -3 306.37 15.40 11 2 -3 284.27 13.10 -11 -2 -3 292.67 13.70 11 2 -3 288.27 11.70 11 -2 3 302.67 14.10 -11 2 3 296.47 13.90 11 -2 3 299.87 13.40 -11 2 3 296.07 13.60 -11 2 -3 288.17 12.90 -11 -2 3 306.77 15.00 -11 -2 3 305.67 12.40 11 -2 -3 299.97 14.00 11 2 3 308.37 11.20 -11 2 -3 293.87 14.40 11 -2 -3 283.47 13.20 11 3 -3 52.69 7.00 11 3 -3 51.59 4.40 -11 -3 -3 62.09 6.20 -11 3 3 51.59 6.20 -11 3 3 50.19 7.20 -11 3 3 49.99 7.10 11 -3 3 53.79 7.30 -11 -3 -3 59.69 8.40 -11 -3 3 42.10 6.40 11 -3 -3 71.59 6.20 -11 3 -3 61.89 6.80 -11 -3 3 52.69 5.50 11 3 3 53.29 3.80 11 -3 -3 50.09 6.60 -11 3 -3 62.19 7.10 11 -4 3 38.10 6.10 11 4 -3 52.49 6.90 -11 -4 -3 37.30 5.40 11 4 -3 44.90 4.80 -11 -4 -3 38.80 6.60 -11 4 3 50.99 7.00 11 4 -3 46.60 6.20 -11 -4 3 47.70 7.40 -11 4 -3 40.00 5.40 -11 4 -3 42.00 6.00 -11 4 -3 46.40 7.00 11 -4 -3 32.90 5.80 11 4 3 38.30 4.00 -11 -4 3 48.20 5.90 11 -4 -3 39.40 5.90 -11 -5 -3 97.99 9.30 11 -5 3 110.19 11.60 11 5 -3 92.29 10.60 -11 5 3 93.99 11.00 11 5 -3 108.49 8.70 -11 5 3 101.49 7.40 -11 -5 -3 117.79 11.60 -11 5 -3 99.59 10.50 -11 -5 3 90.19 11.50 11 -5 -3 112.39 10.10 11 5 3 96.39 6.50 -11 5 -3 102.69 9.40 11 5 3 101.09 6.30 11 -5 -3 86.89 11.70 -11 5 -3 99.79 10.50 -11 -5 3 111.69 8.80 -11 -6 -3 12.20 7.10 -11 6 3 7.20 5.20 11 6 -3 13.00 7.00 -11 -6 -3 5.20 5.40 11 6 -3 4.90 5.40 -11 -6 3 8.30 10.30 -11 6 -3 13.00 5.90 11 6 3 7.90 4.20 -11 6 -3 6.30 7.80 11 6 3 6.70 4.20 -11 -6 3 5.10 5.60 11 -6 -3 0.00 7.60 -11 0 4 1.10 3.10 -11 0 4 -0.30 2.90 -11 0 -4 1.60 1.50 11 0 4 -1.00 1.40 -11 0 -4 -5.10 2.80 11 0 -4 -1.10 1.60 11 0 4 -0.30 3.10 -11 0 4 0.60 2.90 11 0 -4 4.00 2.70 -11 1 4 65.79 6.80 -11 1 4 62.89 6.30 -11 1 4 73.69 6.40 -11 -1 -4 58.49 6.30 11 1 -4 55.09 7.30 -11 -1 -4 58.59 3.30 11 1 -4 55.49 4.90 11 -1 4 65.39 6.40 11 -1 -4 59.59 5.00 11 -1 -4 72.89 6.60 11 1 4 69.59 6.30 -11 1 -4 74.79 6.60 -11 1 -4 66.59 4.80 -11 -1 4 69.59 5.20 11 2 -4 258.87 13.40 11 -2 4 301.47 13.80 -11 -2 -4 268.17 14.60 -11 2 4 295.47 13.40 -11 2 4 299.87 13.10 -11 2 4 299.57 12.60 11 2 -4 236.58 12.40 11 2 -4 259.37 11.30 -11 -2 -4 261.57 13.00 -11 2 -4 249.58 12.10 -11 -2 4 299.07 14.60 11 -2 -4 249.08 12.20 -11 -2 4 300.47 11.40 11 -2 -4 257.67 13.30 -11 2 -4 260.77 13.60 -11 3 4 73.49 6.50 11 3 -4 65.29 6.80 -11 -3 -4 67.19 6.50 11 3 -4 66.79 7.90 11 -3 4 87.19 8.20 -11 -3 -4 71.09 8.90 11 3 -4 63.09 5.40 -11 3 4 89.49 8.10 -11 -3 4 97.19 9.50 11 -3 -4 55.89 7.00 -11 3 -4 72.69 7.30 -11 -3 4 83.69 5.80 11 -3 -4 62.89 7.40 -11 3 -4 59.09 7.90 11 4 -4 59.99 9.30 11 4 -4 66.49 7.10 -11 -4 -4 65.09 7.00 11 -4 4 60.39 9.10 -11 4 4 49.10 6.70 -11 -4 -4 72.29 8.60 11 4 -4 73.39 6.10 -11 4 4 73.49 9.20 -11 4 -4 73.19 9.00 11 -4 -4 68.39 8.60 11 -4 -4 60.89 7.40 -11 4 -4 63.29 7.70 -11 -4 4 55.59 6.10 -11 -4 4 72.69 10.00 -11 4 -4 51.09 7.30 -11 5 4 29.20 4.90 11 -5 4 38.80 7.40 11 5 -4 29.30 5.70 -11 -5 -4 24.60 6.10 -11 5 4 27.30 6.90 11 5 -4 30.70 6.30 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10.30 11 2 -7 121.49 8.50 11 2 -7 111.69 9.00 -11 2 7 121.09 9.90 11 -2 7 116.19 8.70 11 -2 -7 126.19 9.70 11 -2 -7 115.79 7.50 -11 -2 7 135.09 10.90 -11 2 -7 120.49 7.80 -11 2 -7 119.59 9.70 -11 -3 -7 55.59 6.90 11 -3 7 57.89 6.60 -11 -3 -7 65.69 10.00 -11 3 7 63.79 5.50 11 -3 7 48.60 7.00 11 3 -7 68.79 7.20 11 3 -7 57.99 7.40 -11 3 7 50.19 7.10 11 3 -7 52.49 7.20 -11 3 -7 52.09 7.50 11 -3 -7 60.29 7.20 -11 3 -7 65.49 7.50 -11 -3 7 53.09 7.80 -11 3 -7 59.09 8.00 11 -3 -7 69.89 8.60 11 4 -7 92.69 9.30 11 4 -7 87.89 10.30 11 4 -7 84.79 8.80 -11 4 7 88.09 10.90 11 -4 7 83.49 8.60 -11 -4 -7 77.29 8.20 -11 -4 -7 97.19 11.90 11 -4 7 82.79 11.10 -11 4 -7 102.29 9.50 -11 4 -7 95.09 10.30 11 -4 -7 102.79 9.80 11 -4 -7 91.29 9.60 -11 4 -7 87.39 9.20 -11 -4 7 95.79 10.80 -11 -5 -7 11.30 7.20 11 5 -7 27.60 5.70 11 -5 7 18.80 5.10 11 -5 -7 10.10 6.60 -11 5 -7 19.80 5.90 -11 5 -7 10.80 7.00 11 0 8 -0.90 2.40 11 0 -8 0.00 3.00 11 0 -8 2.30 3.90 -11 0 -8 -2.70 4.40 -11 0 -8 -1.60 1.50 11 0 8 0.80 4.50 11 -1 8 75.89 6.10 -11 1 8 71.79 8.30 11 -1 8 75.59 8.70 11 1 -8 57.19 6.90 11 1 -8 56.89 7.50 11 1 -8 53.19 6.70 -11 -1 -8 54.99 7.40 -11 1 8 74.99 7.50 11 -1 -8 46.90 6.90 -11 -1 8 63.69 8.70 -11 1 -8 57.59 8.00 -11 1 -8 46.40 4.80 11 -1 -8 55.39 4.60 -11 2 8 191.88 12.60 11 -2 8 198.88 12.70 -11 -2 -8 185.98 11.90 11 2 -8 191.98 11.00 -11 2 8 201.28 9.70 11 -2 8 189.78 9.90 11 2 -8 193.28 11.50 11 2 -8 187.38 12.50 11 -2 -8 183.68 9.50 -11 2 -8 182.28 13.00 11 -2 -8 201.78 12.40 -11 -2 8 195.28 13.10 -11 2 -8 192.18 10.20 -11 -3 -8 100.89 9.00 11 3 -8 78.49 10.50 11 3 -8 110.19 9.20 -11 3 8 122.09 11.00 11 3 -8 83.19 8.80 -11 3 8 118.19 6.10 11 -3 8 121.69 8.30 11 -3 8 118.29 11.00 -11 -3 -8 111.69 12.10 -11 -3 8 126.09 12.10 11 -3 -8 107.79 9.00 -11 3 -8 105.89 10.90 -11 3 -8 96.79 8.80 11 -3 -8 98.09 10.20 -11 3 -8 92.69 8.50 -11 4 8 42.50 8.30 -11 -4 -8 55.89 7.60 11 4 -8 51.19 7.00 11 4 -8 48.50 8.10 11 -4 8 49.40 8.30 -11 -4 -8 53.49 8.80 11 -4 8 47.70 6.10 -11 4 -8 51.39 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214.28 11.60 12 -3 -2 199.58 11.90 12 -3 -2 215.08 11.90 12 3 2 223.38 9.60 12 4 -2 97.89 7.50 -12 -4 -2 97.29 8.40 -12 -4 -2 98.49 10.90 12 -4 2 90.29 10.30 -12 4 2 80.99 9.40 12 -4 -2 98.49 9.60 -12 -4 2 94.19 8.30 -12 4 -2 96.99 9.30 12 -4 -2 96.99 9.20 -12 4 -2 97.39 10.10 -12 -4 2 103.99 11.40 12 4 2 92.39 6.50 -12 5 2 22.40 6.80 12 5 -2 22.40 5.10 12 -5 2 27.70 7.70 -12 5 2 31.50 5.60 -12 -5 -2 22.10 5.80 -12 -5 -2 20.60 6.70 12 5 2 31.20 4.50 -12 -5 2 30.40 5.90 -12 5 -2 9.00 6.00 -12 -5 2 14.40 6.30 -12 5 -2 15.80 5.40 12 -5 -2 18.70 5.40 -12 5 -2 18.10 6.00 12 -5 -2 17.80 6.00 12 0 -3 693.83 25.80 -12 0 3 630.34 24.80 -12 0 3 640.94 25.10 -12 0 3 627.54 27.00 -12 0 -3 666.03 23.80 12 0 3 634.54 25.40 -12 0 -3 720.13 26.50 12 0 -3 687.03 24.30 12 0 3 670.33 24.20 -12 1 3 298.27 14.50 -12 -1 -3 328.47 15.70 -12 -1 -3 323.07 14.70 12 -1 3 303.27 13.40 12 -1 3 302.37 14.30 12 1 -3 313.57 12.30 -12 -1 -3 317.67 11.70 12 1 -3 327.57 12.60 -12 1 3 298.37 14.80 -12 1 3 297.77 13.90 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11.60 15 2 -7 175.18 13.40 -15 -2 7 208.38 16.90 -15 2 -7 212.08 11.40 15 -2 -7 207.98 11.50 -16 0 0 279.27 16.00 16 0 0 297.27 14.30 -16 0 0 291.17 18.10 16 0 0 296.47 14.90 -16 0 0 277.57 13.30 -16 -1 0 100.79 10.70 16 -1 0 92.19 8.70 16 -1 0 106.29 10.50 16 1 0 100.79 9.70 -16 1 0 93.29 10.60 16 1 0 87.19 6.30 -16 -1 0 90.89 12.70 -16 1 0 99.09 11.00 -16 1 0 94.19 8.30 -16 -2 0 13.90 8.60 16 2 0 11.10 5.90 -16 2 0 6.20 7.30 -16 2 0 7.30 6.50 16 -2 0 4.80 5.90 -16 2 0 10.40 4.60 -16 -2 0 2.80 5.50 16 -2 0 9.20 4.80 -16 3 0 30.80 6.20 -16 -3 0 25.40 9.40 -16 -3 0 39.50 7.60 16 3 0 47.90 7.10 16 -3 0 36.20 7.50 16 -3 0 28.10 7.00 -16 3 0 32.50 7.40 -16 0 -1 69.69 9.10 -16 0 -1 49.99 9.10 -16 0 1 85.69 12.10 -16 0 -1 58.69 6.40 -16 0 1 72.59 7.20 16 0 1 70.99 8.00 16 0 -1 57.29 7.10 -16 0 1 66.69 10.00 16 0 1 90.29 9.50 16 0 -1 63.39 7.90 16 -1 1 166.48 10.90 -16 1 1 147.99 10.30 16 -1 1 152.08 11.20 -16 -1 -1 139.89 14.50 -16 -1 -1 163.08 12.20 16 1 -1 158.48 10.90 -16 1 1 140.39 12.20 -16 1 1 151.18 14.70 16 1 -1 152.68 8.40 -16 1 -1 130.59 9.50 16 -1 -1 146.49 9.90 -16 1 -1 155.18 14.60 -16 -1 1 159.68 11.60 16 -1 -1 151.48 11.90 -16 -1 1 146.59 14.80 -16 1 -1 136.99 12.80 16 1 1 166.68 11.60 16 2 -1 11.80 5.80 -16 2 1 16.40 7.90 16 -2 1 14.40 6.00 16 -2 1 5.70 4.90 -16 -2 -1 14.50 6.10 -16 -2 -1 9.60 7.10 -16 2 1 1.90 4.90 -16 2 1 -0.90 6.20 16 2 -1 8.30 3.20 16 -2 -1 12.10 5.00 -16 -2 1 9.30 8.30 -16 -2 1 6.10 5.50 16 -2 -1 14.30 6.60 16 2 1 11.40 5.80 -16 2 -1 13.00 4.50 -16 2 -1 11.60 6.30 -16 3 1 96.99 11.80 -16 -3 -1 87.09 11.30 16 3 -1 89.99 10.60 -16 3 1 73.89 10.30 -16 3 1 81.29 11.60 16 -3 1 88.59 10.90 -16 -3 -1 86.39 13.40 16 -3 1 74.49 10.60 16 -3 -1 88.09 11.20 -16 -3 1 78.09 12.60 16 -3 -1 77.59 10.40 -16 3 -1 98.69 10.40 -16 -3 1 83.89 11.20 -16 3 -1 85.99 12.30 16 3 1 84.49 10.00 -16 0 -2 200.38 14.50 -16 0 2 243.48 16.60 16 0 -2 226.68 13.50 -16 0 2 241.78 12.10 16 0 -2 207.98 11.30 -16 0 2 192.28 13.30 -16 0 -2 237.08 16.70 16 0 2 231.08 12.90 16 -1 2 158.48 10.90 16 1 -2 155.38 8.80 -16 -1 -2 152.98 14.70 16 1 -2 133.79 11.20 -16 1 2 159.48 14.00 16 -1 2 163.18 11.10 -16 -1 -2 124.49 12.70 -16 1 2 143.39 10.40 -16 1 2 135.49 12.30 -16 1 -2 162.48 9.30 -16 -1 2 137.89 11.90 16 1 2 145.69 10.60 -16 -1 2 134.69 14.50 16 -1 -2 150.38 12.50 -16 1 -2 139.39 12.90 16 -1 -2 149.39 9.80 -16 -2 -2 6.10 6.10 16 -2 2 4.90 5.40 -16 2 2 1.90 6.30 16 2 -2 8.10 3.80 16 2 -2 18.40 5.90 -16 2 2 9.70 5.00 -16 2 2 9.60 7.90 -16 -2 -2 7.50 7.60 16 -2 2 7.00 5.30 -16 -2 2 13.30 6.40 16 -2 -2 12.40 6.10 -16 2 -2 1.80 4.10 16 2 2 17.60 5.20 -16 -2 2 1.50 7.00 16 -2 -2 6.90 4.90 -16 2 -2 10.20 6.80 -16 3 2 15.60 7.50 16 3 -2 11.50 6.10 -16 3 2 25.10 9.50 -16 3 2 19.40 6.50 -16 -3 -2 16.40 7.20 16 -3 2 20.80 7.00 16 -3 2 15.50 6.40 16 -3 -2 16.50 7.00 -16 -3 2 20.00 7.10 -16 -3 2 7.30 12.30 16 -3 -2 19.30 6.60 -16 3 -2 14.80 7.20 16 3 2 28.90 5.80 -16 3 -2 23.20 6.10 16 0 3 31.90 6.10 -16 0 3 36.10 8.40 16 0 -3 33.50 4.90 -16 0 -3 41.60 4.70 -16 0 -3 35.20 8.70 -16 0 3 39.40 7.60 16 0 -3 39.10 7.10 16 0 3 38.70 6.30 -16 0 3 36.80 5.50 -16 0 -3 33.40 7.40 16 -1 3 89.79 10.20 16 1 -3 105.19 10.30 -16 -1 -3 109.29 11.30 -16 1 3 82.69 9.50 -16 -1 -3 115.39 14.90 -16 1 3 96.39 13.10 16 -1 3 78.79 9.70 16 1 -3 117.59 8.50 -16 1 3 89.79 10.40 16 -1 -3 84.09 10.70 16 -1 -3 104.19 8.20 16 1 3 92.79 8.70 -16 1 -3 123.39 11.70 -16 1 -3 95.69 7.70 -16 -1 3 77.29 10.00 -16 2 3 4.80 7.30 16 2 -3 7.80 4.40 -16 -2 -3 -0.30 7.90 -16 2 3 5.50 6.90 -16 2 3 7.70 5.40 16 2 -3 14.20 6.50 -16 -2 -3 3.60 6.00 16 -2 3 9.00 6.00 16 -2 3 5.70 5.50 -16 2 -3 12.80 4.70 16 -2 -3 4.10 5.80 -16 -2 3 2.70 6.10 -16 -2 3 1.90 7.10 -16 2 -3 0.40 6.10 16 2 3 5.10 4.50 16 -2 -3 8.90 4.90 -16 3 3 40.50 9.10 -16 3 3 21.80 7.50 16 3 -3 35.10 4.90 16 3 -3 24.30 7.20 16 -3 3 33.90 10.50 -16 3 3 30.40 8.00 -16 -3 -3 31.80 6.80 16 3 3 33.00 6.40 -16 3 -3 26.10 7.70 16 -3 -3 31.50 7.00 16 -3 -3 35.40 6.80 -16 3 -3 27.80 6.00 16 0 4 204.88 12.80 -16 0 4 186.48 15.30 -16 0 4 199.58 14.70 -16 0 4 185.88 12.20 -16 0 -4 203.28 13.50 -16 0 -4 216.18 9.60 16 0 -4 223.48 14.00 -16 1 4 120.59 10.50 -16 1 4 119.39 12.00 16 1 -4 117.59 11.50 -16 -1 -4 128.29 12.00 16 -1 4 117.99 11.30 16 1 -4 114.69 9.40 -16 1 4 148.99 14.50 -16 -1 -4 136.09 15.50 -16 -1 4 141.99 11.60 16 -1 -4 132.89 8.70 -16 1 -4 125.69 11.90 -16 -1 4 128.39 14.70 -16 1 -4 130.69 8.30 16 -1 -4 130.19 11.30 -16 -2 -4 17.00 9.40 -16 2 4 12.50 6.80 -16 2 4 11.80 8.20 -16 -2 -4 -1.60 5.60 16 2 -4 11.80 5.60 -16 2 4 7.20 5.70 16 -2 4 10.40 5.70 16 2 -4 15.50 5.20 16 -2 -4 17.70 6.80 -16 2 -4 13.40 4.70 -16 2 -4 10.70 6.50 -16 -2 4 11.90 8.50 16 -2 -4 22.50 5.30 -16 -2 4 12.00 6.10 -16 0 5 60.69 9.70 -16 0 5 69.69 10.70 16 0 -5 60.39 8.00 -16 0 5 60.69 8.80 16 0 -5 65.79 6.00 16 0 5 66.79 10.30 -16 0 -5 59.19 5.40 -16 0 -5 79.49 10.70 16 -1 5 129.79 9.00 -16 1 5 127.29 11.20 16 -1 5 102.49 11.90 -16 -1 -5 115.59 16.20 16 1 -5 124.09 12.00 16 1 -5 131.69 10.30 -16 1 5 128.19 12.10 -16 1 5 141.69 14.20 -16 -1 -5 130.89 12.30 16 -1 -5 138.79 9.00 -16 -1 5 132.69 10.90 16 -1 -5 118.89 12.20 -16 1 -5 131.09 12.30 -16 -1 5 118.79 15.60 -16 -2 -5 14.10 6.30 16 2 -5 13.90 6.30 -16 2 5 8.00 7.90 -16 2 5 3.30 6.90 16 2 -5 14.30 5.70 16 -2 5 13.60 4.90 16 -2 -5 12.50 4.80 16 -2 -5 13.10 5.90 -16 -2 5 4.70 8.80 -16 2 -5 5.70 4.40 -16 -2 5 8.30 6.00 16 0 -6 115.39 6.70 -16 0 -6 112.59 6.00 16 0 -6 103.99 10.60 -16 0 6 94.59 14.70 16 0 -6 92.99 11.30 -16 0 -6 135.59 15.50 -16 0 6 92.89 10.90 16 1 -6 127.59 11.10 16 -1 6 101.19 8.70 -16 1 6 120.59 15.00 -16 1 6 113.99 15.30 16 1 -6 142.69 12.20 -16 -1 6 112.59 15.40 16 -1 -6 105.69 12.10 -16 1 -6 109.59 7.50 16 -1 -6 113.29 7.90 -17 0 0 -2.10 7.80 17 0 0 -8.10 5.20 -17 0 0 -2.70 3.80 -17 0 0 0.40 6.50 17 0 0 0.70 4.20 17 -1 0 3.90 6.50 -17 -1 0 4.80 6.70 -17 1 0 -5.10 8.60 -17 -1 0 3.70 7.90 17 1 0 5.70 3.70 -17 1 0 8.40 6.60 -17 1 0 -7.70 4.30 17 1 0 6.20 6.00 17 -1 0 0.20 4.70 17 -2 0 53.09 7.40 -17 2 0 45.80 9.20 -17 2 0 48.40 7.00 17 -2 0 36.70 7.20 -17 -2 0 43.10 8.40 -17 2 0 66.39 11.40 17 2 0 47.50 7.80 -17 0 -1 -2.70 3.80 -17 0 -1 -4.50 8.90 -17 0 1 -15.60 6.50 17 0 -1 11.30 6.40 -17 0 1 1.50 7.70 -17 0 -1 -3.70 6.00 -17 0 1 -1.50 3.80 17 0 -1 -0.10 4.10 17 0 1 0.60 4.40 17 0 1 3.80 5.80 17 1 -1 127.79 11.90 17 -1 1 130.99 11.40 17 -1 1 143.59 11.10 17 1 -1 146.79 8.90 -17 -1 -1 146.19 13.00 -17 1 1 148.69 10.50 -17 1 1 141.09 15.80 -17 1 1 124.49 13.20 -17 -1 -1 140.19 15.90 -17 1 -1 119.49 12.90 17 -1 -1 130.39 10.00 -17 1 -1 139.19 15.80 -17 -1 1 143.69 12.70 17 1 1 145.59 11.90 17 -1 -1 130.69 12.60 -17 1 -1 122.59 9.60 -17 -1 1 144.69 16.40 -17 2 1 108.59 10.20 -17 2 1 96.69 12.50 -17 -2 -1 75.09 11.70 17 -2 1 90.49 11.50 -17 2 1 108.69 15.80 17 -2 1 103.29 10.30 17 2 -1 79.09 10.80 -17 2 -1 92.09 9.10 -17 2 -1 90.09 10.80 17 -2 -1 85.29 10.40 17 -2 -1 97.59 11.50 -17 2 -1 85.79 11.20 -17 -2 1 92.19 17.90 -17 -2 1 107.49 12.10 -17 0 -2 -6.10 3.30 17 0 -2 2.40 4.10 17 0 2 -2.70 5.60 -17 0 2 -8.40 3.80 -17 0 -2 -18.20 8.00 17 0 2 2.60 5.00 17 0 -2 0.00 6.30 -17 0 2 -1.40 7.80 -17 0 2 1.80 6.60 -17 0 -2 -0.60 6.40 17 -1 2 7.00 5.90 17 1 -2 10.50 6.50 -17 1 2 -1.00 8.20 17 -1 2 3.00 6.20 -17 -1 -2 6.10 10.00 -17 -1 -2 15.30 6.60 -17 1 2 -0.10 5.20 -17 1 2 -5.60 6.90 17 -1 -2 2.80 6.10 17 1 2 11.00 6.20 -17 -1 2 18.00 8.70 -17 -1 2 9.70 6.80 -17 1 -2 8.50 8.00 -17 1 -2 3.30 6.70 -17 1 -2 9.20 4.20 17 -1 -2 13.40 5.00 17 2 -2 30.30 7.20 17 -2 2 23.10 7.70 -17 2 2 11.70 7.90 -17 2 2 39.10 9.80 -17 2 2 13.80 6.10 17 -2 2 20.80 6.40 -17 -2 -2 30.30 7.30 17 2 -2 29.20 4.80 -17 2 -2 25.20 7.70 -17 2 -2 18.10 5.20 17 2 2 28.40 6.50 -17 -2 2 18.50 16.60 17 -2 -2 18.50 6.90 17 -2 -2 24.70 6.00 -17 -2 2 36.50 8.00 -17 0 -3 0.50 4.20 17 0 3 1.40 5.10 17 0 -3 -0.70 3.90 -17 0 -3 -5.50 6.00 -17 0 3 -2.80 6.30 17 0 -3 0.20 6.60 -17 0 3 -6.20 4.60 -17 0 3 3.80 8.10 -17 0 -3 -3.80 8.70 -17 1 3 35.70 9.70 17 -1 3 29.40 6.50 -17 -1 -3 48.80 8.20 17 1 -3 42.90 7.70 -17 1 3 30.20 6.20 17 1 -3 49.60 6.10 17 -1 3 33.80 7.00 -17 1 3 45.70 8.40 -17 -1 3 55.19 8.40 -17 1 -3 60.39 9.30 -17 1 -3 44.70 5.60 17 -1 -3 46.20 8.30 17 -1 -3 46.80 5.80 -17 -1 3 32.60 9.70 17 1 3 46.80 6.60 -17 -2 -3 151.98 13.40 17 2 -3 137.29 13.00 -17 2 3 138.69 16.40 -17 2 3 118.39 14.30 -17 2 3 109.29 11.80 17 2 3 139.19 11.10 -17 -2 3 131.69 13.20 -17 2 -3 139.49 10.30 -17 2 -3 151.38 15.20 17 -2 -3 120.69 12.80 17 -2 -3 147.29 11.30 -17 0 4 -8.00 5.00 -17 0 4 -5.70 8.00 17 0 4 -9.30 5.20 17 0 -4 3.50 3.60 17 0 -4 9.50 5.70 -17 0 -4 0.20 6.10 -17 0 -4 1.70 3.10 -17 0 4 -1.30 7.20 17 -1 4 6.80 8.20 -17 1 4 2.60 9.10 17 1 -4 -0.30 6.30 17 1 -4 5.70 5.40 -17 1 4 4.50 7.40 -17 1 4 10.40 5.90 -17 -1 -4 -1.80 6.30 17 -1 -4 -10.90 6.00 -17 1 -4 16.60 7.40 -17 1 -4 9.20 4.10 -17 -1 4 -5.90 8.20 17 -1 -4 3.00 4.30 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 13047 _shelx_res_file ; 3.res created by SHELXL-2014/7 TITL p_b.res in Pca2(1) REM Old TITL p in Pbcm REM SHELXT solution in Pca2(1) REM R1 0.109, Rweak 0.010, Alpha 0.009, Orientation a'=b, b'=a, c'=-c REM Flack x = 0.130 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C11 N O3 F Co CELL 0.71073 14.7269 6.7024 11.7607 90.000 90.000 90.000 ZERR 4.000 0.0005 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, -Y, Z SYMM 1/2-X, Y, 1/2+Z SFAC C H N O CL CO UNIT 44 52 4 12 4 4 TEMP -80.140 SIZE 0.03 0.11 0.13 L.S. 10 ACTA BOND $H rem OMIT -1 51 HTAB O2 O3 EQIV $1 -x+1/2, y, z+1/2 HTAB N1 Cl1_$1 HTAB N1 Cl1 EQIV $2 x, y+1, z HTAB O3 Cl1_$2 EQIV $3 -x+1/2, y, z-1/2 HTAB O3 O1_$3 CONF LIST 6 FMAP 2 TWIN DFIX 0.83 0.02 O2 H2O O3 H3A O3 H3B DFIX 0.89 0.02 N1 H1N N1 H2N PLAN 10 rem EXTI 0.002542 WGHT 0.026200 0.115000 BASF 0.06725 FVAR 0.47872 CO1 6 0.526862 0.108261 0.586784 11.00000 0.01400 0.01243 = 0.02049 0.00085 0.00119 -0.00030 CL1 5 0.234292 -0.071466 0.315407 11.00000 0.02902 0.04239 = 0.02384 -0.00451 -0.00330 0.00659 O1 4 0.297095 0.365063 0.583440 11.00000 0.01769 0.03421 = 0.02189 -0.00037 0.00082 0.00285 O2 4 0.360579 0.383004 0.410557 11.00000 0.01933 0.04874 = 0.01765 0.00228 -0.00220 0.00292 H2O 2 0.307746 0.393135 0.389383 11.00000 0.03730 N1 3 0.338879 -0.122235 0.557334 11.00000 0.02109 0.03247 = 0.02311 -0.00026 -0.00232 -0.00810 H1N 2 0.310290 -0.098788 0.622985 11.00000 0.04066 H2N 2 0.314970 -0.101767 0.488860 11.00000 0.03459 C1 1 0.429778 -0.129116 0.566040 11.00000 0.02343 0.01197 = 0.01866 0.00024 -0.00290 -0.00425 C2 1 0.495164 -0.115297 0.475419 11.00000 0.04001 0.01797 = 0.02049 -0.00370 0.00908 -0.00600 AFIX 43 H2 2 0.481665 -0.092540 0.397502 11.00000 -1.20000 AFIX 0 C3 1 0.583722 -0.141568 0.522420 11.00000 0.02710 0.01520 = 0.04990 -0.00447 0.01036 0.00148 AFIX 43 H3 2 0.639002 -0.148011 0.480950 11.00000 -1.20000 AFIX 0 C4 1 0.574336 -0.156372 0.642520 11.00000 0.02362 0.01447 = 0.05219 0.00722 -0.00801 0.00192 AFIX 43 H4 2 0.622460 -0.174596 0.695299 11.00000 -1.20000 AFIX 0 C5 1 0.480705 -0.139253 0.670084 11.00000 0.02602 0.01770 = 0.01975 0.00444 -0.00214 -0.00404 AFIX 43 H5 2 0.455980 -0.135200 0.744657 11.00000 -1.20000 AFIX 0 C6 1 0.538637 0.368054 0.496883 11.00000 0.01576 0.01549 = 0.02591 0.00200 0.00316 -0.00275 AFIX 43 H6 2 0.541320 0.379114 0.416421 11.00000 -1.20000 AFIX 0 C7 1 0.613648 0.349370 0.571732 11.00000 0.01524 0.01580 = 0.04364 0.00098 0.00412 -0.00285 AFIX 43 H7 2 0.675741 0.347215 0.549870 11.00000 -1.20000 AFIX 0 C8 1 0.580644 0.334480 0.684341 11.00000 0.02071 0.01801 = 0.02961 -0.00418 -0.00767 0.00009 AFIX 43 H8 2 0.616613 0.319776 0.750870 11.00000 -1.20000 AFIX 0 C9 1 0.484463 0.345320 0.680674 11.00000 0.01949 0.01690 = 0.02181 -0.00375 -0.00321 0.00201 AFIX 43 H9 2 0.444853 0.339052 0.744330 11.00000 -1.20000 AFIX 0 C10 1 0.457706 0.367149 0.565429 11.00000 0.01683 0.01284 = 0.01878 -0.00089 0.00021 0.00164 C11 1 0.363219 0.371905 0.522093 11.00000 0.01947 0.01485 = 0.01859 0.00010 -0.00211 0.00293 O3 4 0.207651 0.468875 0.315929 11.00000 0.02826 0.04148 = 0.02373 -0.00475 -0.00540 -0.00089 H3A 2 0.211645 0.589645 0.309414 11.00000 0.03610 H3B 2 0.209693 0.427894 0.250984 11.00000 0.02431 HKLF 4 REM p_b.res in Pca2(1) REM R1 = 0.0195 for 2099 Fo > 4sig(Fo) and 0.0206 for all 2163 data REM 175 parameters refined using 6 restraints END WGHT 0.0262 0.1150 REM Highest difference peak 0.495, deepest hole -0.312, 1-sigma level 0.048 Q1 1 0.5268 0.5989 0.5881 11.00000 0.05 0.50 Q2 1 0.5787 -0.0953 0.5836 11.00000 0.05 0.18 Q3 1 0.1294 0.5826 0.3125 11.00000 0.05 0.18 Q4 1 0.2673 0.1020 0.4123 11.00000 0.05 0.16 Q5 1 0.2351 0.3968 0.3074 11.00000 0.05 0.15 Q6 1 0.3289 -0.3583 0.5857 11.00000 0.05 0.14 Q7 1 0.5800 0.3962 0.6413 11.00000 0.05 0.14 Q8 1 0.5745 0.3894 0.5379 11.00000 0.05 0.14 Q9 1 0.4661 0.3688 0.6362 11.00000 0.05 0.14 Q10 1 0.4270 0.5447 0.4837 11.00000 0.05 0.14 ; _shelx_res_checksum 52283 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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 Co Co1 0.52686(2) 0.10826(4) 0.58678(3) 0.01564(11) Uani d 1 Cl Cl1 0.23429(5) -0.07147(13) 0.31541(7) 0.0317(2) Uani d 1 O O1 0.29710(11) 0.3651(3) 0.5834(2) 0.0246(4) Uani d 1 O O2 0.36058(15) 0.3830(4) 0.41056(19) 0.0286(5) Uani d 1 H H2O 0.3077(19) 0.393(6) 0.389(4) 0.037(12) Uiso d 1 N N1 0.33888(18) -0.1222(4) 0.5573(2) 0.0256(6) Uani d 1 H H1N 0.310(3) -0.099(5) 0.623(2) 0.041(12) Uiso d 1 H H2N 0.315(2) -0.102(5) 0.489(2) 0.035(10) Uiso d 1 C C1 0.42978(19) -0.1291(4) 0.5660(2) 0.0180(6) Uani d 1 C C2 0.4952(3) -0.1153(5) 0.4754(3) 0.0262(8) Uani d 1 H H2 0.4817 -0.0925 0.3975 0.031 Uiso calc 1 C C3 0.5837(3) -0.1416(6) 0.5224(4) 0.0307(9) Uani d 1 H H3 0.6390 -0.1480 0.4810 0.037 Uiso calc 1 C C4 0.5743(2) -0.1564(5) 0.6425(3) 0.0301(8) Uani d 1 H H4 0.6225 -0.1746 0.6953 0.036 Uiso calc 1 C C5 0.4807(2) -0.1393(5) 0.6701(3) 0.0212(8) Uani d 1 H H5 0.4560 -0.1352 0.7447 0.025 Uiso calc 1 C C6 0.5386(2) 0.3681(4) 0.4969(3) 0.0191(6) Uani d 1 H H6 0.5413 0.3791 0.4164 0.023 Uiso calc 1 C C7 0.61365(18) 0.3494(4) 0.5717(3) 0.0249(7) Uani d 1 H H7 0.6757 0.3472 0.5499 0.030 Uiso calc 1 C C8 0.5806(2) 0.3345(5) 0.6843(3) 0.0228(6) Uani d 1 H H8 0.6166 0.3198 0.7509 0.027 Uiso calc 1 C C9 0.4845(2) 0.3453(5) 0.6807(3) 0.0194(6) Uani d 1 H H9 0.4449 0.3391 0.7443 0.023 Uiso calc 1 C C10 0.45771(18) 0.3671(4) 0.5654(2) 0.0161(7) Uani d 1 C C11 0.3632(2) 0.3719(4) 0.5221(2) 0.0176(6) Uani d 1 O O3 0.20765(15) 0.4689(4) 0.3159(2) 0.0312(5) Uani d 1 H H3A 0.212(3) 0.590(4) 0.309(4) 0.036(12) Uiso d 1 H H3B 0.210(2) 0.428(5) 0.251(2) 0.024(10) 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 Co1 0.01400(17) 0.01243(17) 0.02049(19) -0.00030(13) 0.00119(18) 0.0009(2) Cl1 0.0290(5) 0.0424(4) 0.0238(4) 0.0066(3) -0.0033(3) -0.0045(3) O1 0.0177(8) 0.0342(10) 0.0219(9) 0.0028(8) 0.0008(12) -0.0004(11) O2 0.0193(11) 0.0487(15) 0.0177(11) 0.0029(10) -0.0022(9) 0.0023(9) N1 0.0211(13) 0.0325(15) 0.0231(16) -0.0081(11) -0.0023(10) -0.0003(10) C1 0.0234(14) 0.0120(12) 0.0187(18) -0.0042(10) -0.0029(12) 0.0002(11) C2 0.0400(18) 0.0180(17) 0.0205(17) -0.0060(14) 0.0091(16) -0.0037(13) C3 0.0271(19) 0.0152(18) 0.050(2) 0.0015(14) 0.0104(16) -0.0045(15) C4 0.0236(18) 0.0145(17) 0.052(2) 0.0019(15) -0.0080(16) 0.0072(16) C5 0.0260(18) 0.0177(17) 0.0197(18) -0.0040(12) -0.0021(13) 0.0044(12) C6 0.0158(15) 0.0155(16) 0.0259(16) -0.0028(12) 0.0032(12) 0.0020(12) C7 0.0152(12) 0.0158(12) 0.044(2) -0.0029(10) 0.0041(15) 0.0010(15) C8 0.0207(15) 0.0180(14) 0.0296(16) 0.0001(13) -0.0077(12) -0.0042(12) C9 0.0195(16) 0.0169(14) 0.0218(16) 0.0020(12) -0.0032(12) -0.0038(12) C10 0.0168(12) 0.0128(12) 0.019(2) 0.0016(10) 0.0002(12) -0.0009(11) C11 0.0195(14) 0.0149(14) 0.0186(15) 0.0029(11) -0.0021(11) 0.0001(10) O3 0.0283(12) 0.0415(16) 0.0237(12) -0.0009(11) -0.0054(11) -0.0047(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 C4 Co1 C3 41.29(13) C4 Co1 C10 165.32(14) C3 Co1 C10 150.63(14) C4 Co1 C9 128.13(14) C3 Co1 C9 168.22(15) C10 Co1 C9 40.91(12) C4 Co1 C5 40.98(16) C3 Co1 C5 69.17(14) C10 Co1 C5 125.96(13) C9 Co1 C5 105.78(15) C4 Co1 C2 69.06(16) C3 Co1 C2 41.12(17) C10 Co1 C2 115.67(14) C9 Co1 C2 148.29(15) C5 Co1 C2 68.66(15) C4 Co1 C6 152.63(14) C3 Co1 C6 118.50(14) C10 Co1 C6 41.38(11) C9 Co1 C6 68.98(12) C5 Co1 C6 165.42(13) C2 Co1 C6 108.20(14) C4 Co1 C8 109.46(15) C3 Co1 C8 131.28(15) C10 Co1 C8 68.42(12) C9 Co1 C8 40.56(12) C5 Co1 C8 117.29(15) C2 Co1 C8 169.83(14) C6 Co1 C8 68.19(12) C4 Co1 C7 120.07(14) C3 Co1 C7 111.08(14) C10 Co1 C7 68.35(11) C9 Co1 C7 68.01(13) C5 Co1 C7 151.79(13) C2 Co1 C7 131.23(15) C6 Co1 C7 40.34(13) C8 Co1 C7 40.07(14) C4 Co1 C1 67.48(13) C3 Co1 C1 67.67(13) C10 Co1 C1 106.55(11) C9 Co1 C1 115.79(11) C5 Co1 C1 39.94(12) C2 Co1 C1 40.01(13) C6 Co1 C1 128.84(12) C8 Co1 C1 149.60(12) C7 Co1 C1 168.03(13) C11 O2 H2O 110(3) C1 N1 H1N 114(3) C1 N1 H2N 118(2) H1N N1 H2N 125(4) N1 C1 C5 125.9(3) N1 C1 C2 127.4(3) C5 C1 C2 106.5(3) N1 C1 Co1 130.2(2) C5 C1 Co1 65.91(16) C2 C1 Co1 65.92(18) C3 C2 C1 108.5(3) C3 C2 Co1 68.5(2) C1 C2 Co1 74.07(18) C3 C2 H2 125.8 C1 C2 H2 125.8 Co1 C2 H2 123.2 C4 C3 C2 107.7(4) C4 C3 Co1 69.2(2) C2 C3 Co1 70.4(2) C4 C3 H3 126.1 C2 C3 H3 126.1 Co1 C3 H3 125.8 C5 C4 C3 108.4(4) C5 C4 Co1 70.53(19) C3 C4 Co1 69.5(2) C5 C4 H4 125.8 C3 C4 H4 125.8 Co1 C4 H4 125.8 C4 C5 C1 108.4(3) C4 C5 Co1 68.49(18) C1 C5 Co1 74.15(18) C4 C5 H5 125.8 C1 C5 H5 125.8 Co1 C5 H5 123.2 C7 C6 C10 107.3(3) C7 C6 Co1 70.72(17) C10 C6 Co1 68.68(16) C7 C6 H6 126.4 C10 C6 H6 126.4 Co1 C6 H6 125.8 C8 C7 C6 108.7(3) C8 C7 Co1 69.65(17) C6 C7 Co1 68.94(16) C8 C7 H7 125.7 C6 C7 H7 125.7 Co1 C7 H7 127.3 C7 C8 C9 108.1(3) C7 C8 Co1 70.27(17) C9 C8 Co1 68.71(17) C7 C8 H8 125.9 C9 C8 H8 125.9 Co1 C8 H8 126.6 C8 C9 C10 108.1(3) C8 C9 Co1 70.73(17) C10 C9 Co1 69.34(17) C8 C9 H9 125.9 C10 C9 H9 125.9 Co1 C9 H9 125.6 C9 C10 C6 107.8(2) C9 C10 C11 126.3(3) C6 C10 C11 125.8(3) C9 C10 Co1 69.76(16) C6 C10 Co1 69.94(16) C11 C10 Co1 122.18(18) O1 C11 O2 124.9(3) O1 C11 C10 123.3(3) O2 C11 C10 111.8(3) H3A O3 H3B 104(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 C4 2.016(4) Co1 C3 2.019(4) Co1 C10 2.028(3) Co1 C9 2.033(3) Co1 C5 2.043(3) Co1 C2 2.044(4) Co1 C6 2.044(3) Co1 C8 2.060(3) Co1 C7 2.068(3) Co1 C1 2.153(3) O1 C11 1.213(4) O2 C11 1.314(4) O2 H2O 0.82(2) N1 C1 1.343(4) N1 H1N 0.89(2) N1 H2N 0.89(2) C1 C5 1.437(4) C1 C2 1.439(5) C2 C3 1.427(6) C2 H2 0.9500 C3 C4 1.423(5) C3 H3 0.9500 C4 C5 1.421(5) C4 H4 0.9500 C5 H5 0.9500 C6 C7 1.418(4) C6 C10 1.439(4) C6 H6 0.9500 C7 C8 1.414(5) C7 H7 0.9500 C8 C9 1.419(4) C8 H8 0.9500 C9 C10 1.419(4) C9 H9 0.9500 C10 C11 1.482(4) O3 H3A 0.82(2) O3 H3B 0.81(2) 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 O2 H2O O3 . 0.82(2) 1.78(3) 2.577(3) 163(4) N1 H1N Cl1 4 0.89(2) 2.36(3) 3.239(3) 166(4) N1 H2N Cl1 . 0.89(2) 2.37(3) 3.253(3) 172(3) O3 H3A Cl1 1_565 0.82(2) 2.30(2) 3.106(3) 172(4) O3 H3B O1 4_554 0.81(2) 2.02(3) 2.822(4) 171(3) 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 N1 C1 C2 C3 -176.6(3) C5 C1 C2 C3 7.0(3) Co1 C1 C2 C3 60.2(2) N1 C1 C2 Co1 123.2(3) C5 C1 C2 Co1 -53.2(2) C1 C2 C3 C4 -4.4(4) Co1 C2 C3 C4 59.4(3) C1 C2 C3 Co1 -63.7(2) C2 C3 C4 C5 -0.1(5) Co1 C3 C4 C5 60.0(3) C2 C3 C4 Co1 -60.1(3) C3 C4 C5 C1 4.5(4) Co1 C4 C5 C1 63.9(2) C3 C4 C5 Co1 -59.4(3) N1 C1 C5 C4 176.5(3) C2 C1 C5 C4 -7.0(3) Co1 C1 C5 C4 -60.2(2) N1 C1 C5 Co1 -123.3(3) C2 C1 C5 Co1 53.22(19) C10 C6 C7 C8 0.7(3) Co1 C6 C7 C8 -58.5(2) C10 C6 C7 Co1 59.19(19) C6 C7 C8 C9 -0.4(3) Co1 C7 C8 C9 -58.5(2) C6 C7 C8 Co1 58.0(2) C7 C8 C9 C10 0.0(3) Co1 C8 C9 C10 -59.5(2) C7 C8 C9 Co1 59.4(2) C8 C9 C10 C6 0.5(3) Co1 C9 C10 C6 -59.84(19) C8 C9 C10 C11 176.0(2) Co1 C9 C10 C11 115.7(3) C8 C9 C10 Co1 60.3(2) C7 C6 C10 C9 -0.8(3) Co1 C6 C10 C9 59.7(2) C7 C6 C10 C11 -176.3(2) Co1 C6 C10 C11 -115.8(3) C7 C6 C10 Co1 -60.49(19) C9 C10 C11 O1 3.0(4) C6 C10 C11 O1 177.8(3) Co1 C10 C11 O1 90.4(3) C9 C10 C11 O2 -176.6(3) C6 C10 C11 O2 -1.8(4) Co1 C10 C11 O2 -89.2(3) _cod_database_fobs_code 2242809