#------------------------------------------------------------------------------ #$Date: 2020-03-04 08:13:49 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248737 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557436.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_1557436 loop_ _publ_author_name 'Giltzau, Niels Ole' 'K\"ockerling, Martin' _publ_section_title ; Bis(N-adamantyl-N′-ethylimidazolium) tetrabromidomanganate(II) ; _journal_coeditor_code WM4124 _journal_issue 3 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314620002618 _journal_volume 5 _journal_year 2020 _chemical_formula_iupac '(C15 H23 N2)2 [Mn Br4]' _chemical_formula_moiety '2(C15 H23 N2 +), Br4 Mn 2-' _chemical_formula_sum 'C30 H46 Br4 Mn N4' _chemical_formula_weight 837.29 _chemical_name_systematic ; Bis(N-adamantyl-N'-ethylimidazolium) tetrabromidomanganate(II) ; _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'ciftab-2016 (M. K\"ockerling, 2016)' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.0200(10) _cell_length_b 18.7420(10) _cell_length_c 19.7400(10) _cell_measurement_reflns_used 9879 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 28.305 _cell_measurement_theta_min 2.3525 _cell_volume 6666.8(6) _computing_cell_refinement ; SAINT (Bruker, 2017) ; _computing_data_collection ; APEX2 (Bruker, 2017) ; _computing_data_reduction ; SAINT (Bruker, 2017) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2019) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX KappaII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_unetI/netI 0.0230 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 182157 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.061 _exptl_absorpt_coefficient_mu 5.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method none _exptl_crystal_description 'irregular block' _exptl_crystal_F_000 3352 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.716 _refine_diff_density_min -0.504 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5883 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.207 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0269 _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^)+(0.0237P)^2^+8.9922P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.0661 _reflns_number_gt 5029 _reflns_number_total 5883 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm4124sup1.cif _cod_data_source_block I _cod_original_cell_volume 6666.6(7) _cod_database_code 1557436 _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 0.393 _shelx_estimated_absorpt_t_max 0.780 _shelx_hkl_file ; -1 0 0 0.03 0.03 -2 0 0 0.24 0.08 -2 0 0 -0.08 0.07 -2 0 0 0.13 0.11 -2 0 0 -0.09 0.06 -2 0 0 0.03 0.09 2 0 0 0.45 0.10 2 0 0 0.21 0.10 2 0 0 0.09 0.10 2 0 0 0.14 0.08 -3 0 0 0.29 0.37 -3 0 0 -0.30 0.30 -3 0 0 0.14 0.22 -3 0 0 0.94 0.35 -3 0 0 -0.23 0.39 -3 0 0 0.51 0.31 3 0 0 0.57 0.41 3 0 0 1.14 0.38 3 0 0 0.43 0.31 3 0 0 0.99 0.27 3 0 0 0.42 0.37 3 0 0 0.16 0.31 -4 0 0 118.21 7.83 -4 0 0 108.44 7.85 -4 0 0 112.91 7.88 -4 0 0 111.75 7.87 -4 0 0 111.91 7.79 -4 0 0 108.32 7.84 4 0 0 102.98 7.81 4 0 0 108.18 7.82 4 0 0 99.14 7.84 4 0 0 117.22 7.86 4 0 0 110.55 7.88 4 0 0 105.02 7.83 4 0 0 106.52 7.84 -5 0 0 -0.56 0.46 -5 0 0 -0.10 0.37 -5 0 0 -0.16 0.39 -5 0 0 -1.21 0.57 -5 0 0 0.29 0.30 5 0 0 0.18 0.54 5 0 0 0.97 0.44 5 0 0 0.65 0.49 5 0 0 0.17 0.53 5 0 0 -0.03 0.45 5 0 0 -0.20 0.44 -6 0 0 291.43 22.51 -6 0 0 318.56 22.42 -6 0 0 304.35 22.49 -6 0 0 329.03 22.41 -6 0 0 328.09 22.51 6 0 0 302.50 22.48 6 0 0 321.38 22.47 6 0 0 289.09 22.51 6 0 0 358.45 22.53 -7 0 0 -0.70 0.44 -7 0 0 -1.19 0.59 -7 0 0 -0.07 0.34 -7 0 0 0.09 0.33 -7 0 0 -0.66 0.54 -7 0 0 -0.31 0.54 7 0 0 0.45 0.62 7 0 0 -0.54 0.51 7 0 0 -0.62 0.45 -8 0 0 110.26 7.62 -8 0 0 114.22 7.79 -8 0 0 99.84 7.84 -8 0 0 97.83 7.76 -8 0 0 112.30 7.64 -8 0 0 111.05 7.66 -8 0 0 98.43 7.76 8 0 0 108.45 7.75 8 0 0 120.83 7.82 8 0 0 91.70 7.78 -9 0 0 -1.18 0.86 -9 0 0 1.13 0.35 -9 0 0 -0.80 0.63 -9 0 0 0.43 0.56 -9 0 0 0.96 0.43 -9 0 0 -0.12 0.77 -9 0 0 0.29 0.42 9 0 0 -0.85 0.86 9 0 0 0.11 0.77 9 0 0 0.80 0.66 -10 0 0 69.06 4.75 -10 0 0 58.26 4.86 -10 0 0 55.93 4.71 -10 0 0 57.78 4.74 -10 0 0 65.28 4.53 -10 0 0 64.96 4.58 -10 0 0 62.36 4.50 10 0 0 60.39 4.65 10 0 0 68.93 4.78 10 0 0 57.19 4.86 -11 0 0 0.01 0.50 -11 0 0 -0.31 0.67 -11 0 0 0.76 0.40 -11 0 0 -0.42 1.07 -11 0 0 0.58 0.79 -11 0 0 -0.39 0.86 11 0 0 -1.11 0.89 11 0 0 -1.11 1.04 11 0 0 0.93 0.77 -12 0 0 136.53 10.05 -12 0 0 140.94 10.38 -12 0 0 146.23 10.25 -12 0 0 131.10 10.22 -12 0 0 141.19 10.26 12 0 0 143.06 10.20 12 0 0 130.46 10.28 12 0 0 150.61 10.26 -13 0 0 0.63 0.79 -13 0 0 0.22 0.83 -13 0 0 0.67 0.57 -13 0 0 1.42 0.93 -13 0 0 0.53 1.00 13 0 0 0.78 0.93 13 0 0 0.76 1.08 13 0 0 0.42 0.94 -14 0 0 96.98 7.09 -14 0 0 95.77 7.14 -14 0 0 93.99 6.89 -14 0 0 98.47 7.37 -14 0 0 86.85 7.13 14 0 0 88.94 7.45 14 0 0 97.99 7.10 14 0 0 93.48 7.32 14 0 0 100.59 7.21 -15 0 0 -0.26 0.90 -15 0 0 -0.93 1.47 -15 0 0 1.56 1.17 -15 0 0 -0.71 0.56 -15 0 0 1.78 1.15 15 0 0 0.20 0.98 15 0 0 0.43 0.92 15 0 0 2.32 1.49 15 0 0 1.00 1.51 -16 0 0 35.38 2.55 -16 0 0 31.20 3.16 -16 0 0 31.95 2.63 -16 0 0 32.55 3.05 -16 0 0 31.51 2.87 -16 0 0 34.05 3.51 16 0 0 33.86 3.10 16 0 0 34.84 3.04 16 0 0 36.23 3.65 16 0 0 33.97 3.47 -17 0 0 0.12 1.18 -17 0 0 -1.01 1.66 -17 0 0 -0.09 1.15 -17 0 0 -1.19 1.18 17 0 0 2.00 1.32 17 0 0 -0.60 1.15 17 0 0 -0.47 1.24 17 0 0 1.19 1.34 -18 0 0 119.78 9.54 -18 0 0 133.09 9.70 -18 0 0 144.00 9.99 -18 0 0 124.36 9.62 18 0 0 127.20 9.77 18 0 0 134.13 9.61 18 0 0 128.71 9.64 18 0 0 128.51 10.09 -19 0 0 0.43 1.14 -19 0 0 0.20 1.10 -19 0 0 2.31 1.54 -19 0 0 0.94 0.98 19 0 0 0.69 1.19 19 0 0 4.01 1.58 19 0 0 1.04 1.76 19 0 0 2.63 1.94 -20 0 0 1.58 1.18 -20 0 0 0.51 1.37 -20 0 0 0.54 1.99 -20 0 0 1.29 1.19 20 0 0 5.01 1.61 20 0 0 2.03 1.29 20 0 0 2.29 2.03 20 0 0 2.62 1.93 -21 0 0 -1.02 1.27 -21 0 0 -0.35 1.36 -21 0 0 -2.03 2.03 -21 0 0 -0.78 1.31 21 0 0 0.46 1.64 21 0 0 0.42 1.54 21 0 0 -1.71 1.58 21 0 0 0.79 1.44 21 0 1 -0.26 2.00 21 0 1 1.40 1.61 21 0 1 -0.11 1.89 21 0 1 -2.74 1.46 -21 0 -1 -1.88 2.08 -21 0 -1 -1.47 1.36 -21 0 -1 -4.03 1.28 20 0 1 1.60 1.92 20 0 1 0.33 1.77 20 0 1 -1.52 1.41 20 0 1 1.46 1.54 -20 0 -1 -0.24 0.98 -20 0 -1 -2.94 1.15 -20 0 -1 -2.57 1.91 -20 0 -1 -0.21 1.36 19 0 1 0.24 1.39 19 0 1 0.00 1.26 19 0 1 -1.50 1.18 19 0 1 0.07 1.36 -19 0 -1 -0.56 1.45 -19 0 -1 -0.43 1.34 -19 0 -1 -2.02 1.25 -19 0 -1 -2.04 1.13 18 0 1 0.23 1.36 18 0 1 -0.57 1.18 18 0 1 -0.09 1.68 18 0 1 -0.64 1.62 -18 0 -1 -2.13 1.28 -18 0 -1 -1.04 1.14 -18 0 -1 0.75 1.29 -18 0 -1 -0.47 1.29 17 0 1 0.43 1.52 17 0 1 0.49 1.29 17 0 1 -0.50 1.11 17 0 1 0.77 1.15 -17 0 -1 -1.31 0.89 -17 0 -1 0.12 1.69 -17 0 -1 0.02 1.08 -17 0 -1 -0.95 1.18 16 0 1 0.25 1.26 16 0 1 -0.48 1.18 16 0 1 -0.69 1.43 -16 0 -1 -3.41 1.54 -16 0 -1 -1.06 1.09 -16 0 -1 -1.59 0.96 -16 0 -1 -0.60 1.05 -16 0 -1 -1.13 0.45 15 0 1 -0.74 1.02 15 0 1 -1.17 1.18 15 0 1 -0.50 1.39 -15 0 -1 -2.42 1.47 -15 0 -1 0.04 0.49 -15 0 -1 -1.38 0.41 -15 0 -1 1.18 0.44 -15 0 -1 -0.51 1.03 -15 0 -1 -1.63 0.94 -15 0 -1 0.80 0.84 14 0 1 0.51 1.11 14 0 1 -1.06 0.94 14 0 1 -0.42 0.99 -14 0 -1 0.06 0.79 -14 0 -1 -1.45 1.41 -14 0 -1 -0.53 0.42 -14 0 -1 -0.20 1.17 -14 0 -1 0.72 0.47 -14 0 -1 -1.01 0.77 13 0 1 -0.82 1.20 13 0 1 -1.11 0.73 13 0 1 -0.01 0.93 -13 0 -1 -0.91 0.84 -13 0 -1 -1.19 1.26 -13 0 -1 0.37 0.76 -13 0 -1 1.46 0.41 -13 0 -1 -1.45 0.42 -13 0 -1 -0.25 0.98 -13 0 -1 1.30 0.47 12 0 1 -1.40 0.80 12 0 1 -1.10 0.94 12 0 1 -0.92 0.85 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0.08 -2 0 1 0.23 0.13 -2 0 1 0.10 0.13 -2 0 1 -0.13 0.11 -2 0 1 0.06 0.14 -2 0 1 -0.09 0.06 2 0 -1 -0.04 0.07 2 0 -1 -0.29 0.12 2 0 -1 -0.12 0.13 2 0 -1 0.22 0.12 2 0 -1 0.16 0.13 2 0 -1 0.00 0.09 2 0 -1 0.14 0.09 -3 0 1 -0.30 0.31 -3 0 1 -0.38 0.25 -3 0 1 0.37 0.28 -3 0 1 0.25 0.27 -3 0 1 0.64 0.35 -3 0 1 0.08 0.32 -3 0 1 0.18 0.23 -3 0 1 0.40 0.32 3 0 -1 0.33 0.27 3 0 -1 0.06 0.41 3 0 -1 0.32 0.43 3 0 -1 0.34 0.32 3 0 -1 0.13 0.29 3 0 -1 -0.08 0.26 3 0 -1 -0.03 0.23 3 0 -1 -0.19 0.34 -4 0 1 -0.30 0.34 -4 0 1 -0.94 0.52 -4 0 1 0.23 0.32 -4 0 1 0.69 0.44 -4 0 1 0.38 0.36 -4 0 1 0.56 0.37 -4 0 1 0.38 0.42 4 0 -1 0.26 0.34 4 0 -1 0.63 0.39 4 0 -1 0.37 0.53 4 0 -1 0.05 0.29 4 0 -1 -0.26 0.34 4 0 -1 0.04 0.41 4 0 -1 0.34 0.30 4 0 -1 0.17 0.50 -5 0 1 0.16 0.48 -5 0 1 0.93 0.41 -5 0 1 -0.23 0.42 -5 0 1 -0.22 0.65 -5 0 1 0.20 0.41 5 0 -1 0.36 0.44 5 0 -1 0.11 0.46 5 0 -1 -0.40 0.63 5 0 -1 0.53 0.45 5 0 -1 0.11 0.57 5 0 -1 0.32 0.38 -6 0 1 0.49 0.41 -6 0 1 -0.19 0.50 -6 0 1 -0.49 0.50 -6 0 1 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0.54 -7 2 0 -0.08 0.32 -7 2 0 -0.76 0.72 -7 2 0 -1.18 0.66 -7 2 0 -0.12 0.38 -7 2 0 -0.12 0.39 6 -2 0 47.72 3.39 6 -2 0 48.42 3.30 6 -2 0 43.48 3.42 6 -2 0 43.94 3.45 -6 2 0 43.32 3.39 -6 2 0 38.12 3.48 -6 2 0 47.70 3.33 -6 2 0 44.39 3.40 -6 2 0 46.89 3.43 -6 2 0 48.82 3.29 5 -2 0 0.44 0.53 5 -2 0 0.10 0.23 5 -2 0 0.37 0.48 5 -2 0 0.22 0.57 5 -2 0 -0.21 0.32 5 -2 0 0.27 0.40 -5 2 0 0.14 0.25 -5 2 0 -0.03 0.31 -5 2 0 -1.02 0.54 -5 2 0 0.35 0.35 -5 2 0 -1.21 0.56 -5 2 0 -0.73 0.51 4 -2 0 96.08 7.24 4 -2 0 93.77 7.16 4 -2 0 98.64 7.18 4 -2 0 100.63 7.28 4 -2 0 108.42 7.26 4 -2 0 100.68 7.25 4 -2 0 103.08 7.20 4 -2 0 99.12 7.24 -4 2 0 103.52 7.24 -4 2 0 101.20 7.20 -4 2 0 101.64 7.17 -4 2 0 110.04 7.30 -4 2 0 87.23 7.26 -4 2 0 103.04 7.24 -4 2 0 104.34 7.24 -4 2 0 103.39 7.19 3 -2 0 0.10 0.28 3 -2 0 0.32 0.38 3 -2 0 -0.01 0.24 3 -2 0 -0.20 0.16 3 -2 0 -0.21 0.22 3 -2 0 0.15 0.38 3 -2 0 -0.08 0.34 3 -2 0 -0.19 0.25 -3 2 0 -0.29 0.36 -3 2 0 0.06 0.26 -3 2 0 0.02 0.24 -3 2 0 -0.53 0.30 -3 2 0 -0.03 0.16 -3 2 0 -0.20 0.28 -3 2 0 -0.16 0.23 -3 2 0 -0.07 0.26 -3 2 0 0.13 0.18 2 -2 0 1.95 0.24 2 -2 0 3.36 0.37 2 -2 0 2.93 0.39 2 -2 0 2.82 0.37 2 -2 0 3.08 0.33 2 -2 0 1.93 0.26 2 -2 0 1.96 0.28 2 -2 0 2.83 0.27 -2 2 0 2.92 0.31 -2 2 0 2.88 0.32 -2 2 0 1.90 0.34 -2 2 0 2.61 0.28 -2 2 0 1.63 0.24 -2 2 0 1.24 0.32 -2 2 0 1.96 0.34 -2 2 0 2.83 0.28 1 -2 0 -0.01 0.07 1 -2 0 -0.05 0.08 1 -2 0 -0.01 0.07 1 -2 0 -0.05 0.04 1 -2 0 0.04 0.07 1 -2 0 -0.02 0.08 1 -2 0 -0.14 0.10 1 -2 0 0.02 0.06 1 -2 0 0.02 0.10 -1 2 0 -0.07 0.06 -1 2 0 0.01 0.05 -1 2 0 0.00 0.09 -1 2 0 0.00 0.08 -1 2 0 0.04 0.08 -1 2 0 -0.05 0.09 -1 2 0 0.02 0.06 -1 2 0 -0.03 0.05 -1 2 0 -0.01 0.09 -1 2 0 -0.17 0.09 0 2 0 -0.02 0.04 0 2 0 -0.03 0.03 -1 -2 0 0.02 0.10 -1 -2 0 0.02 0.05 -1 -2 0 0.02 0.06 -1 -2 0 -0.05 0.08 -1 -2 0 -0.10 0.07 -1 -2 0 -0.03 0.06 -1 -2 0 0.03 0.07 -1 -2 0 -0.09 0.07 -1 -2 0 -0.01 0.08 -1 -2 0 0.01 0.07 1 2 0 -0.09 0.06 1 2 0 0.02 0.06 1 2 0 0.01 0.05 1 2 0 0.04 0.06 1 2 0 -0.07 0.10 1 2 0 -0.10 0.09 1 2 0 0.05 0.09 1 2 0 -0.07 0.08 1 2 0 -0.05 0.04 -2 -2 0 1.80 0.26 -2 -2 0 1.82 0.21 -2 -2 0 2.78 0.33 -2 -2 0 2.59 0.23 -2 -2 0 1.78 0.29 -2 -2 0 1.98 0.28 -2 -2 0 1.93 0.24 -2 -2 0 1.73 0.29 2 2 0 1.62 0.25 2 2 0 1.64 0.25 2 2 0 2.22 0.28 2 2 0 1.67 0.29 2 2 0 2.22 0.34 2 2 0 2.00 0.21 2 2 0 1.68 0.28 2 2 0 2.45 0.31 -3 -2 0 0.25 0.26 -3 -2 0 0.18 0.24 -3 -2 0 0.14 0.20 -3 -2 0 0.25 0.22 -3 -2 0 0.17 0.16 -3 -2 0 0.08 0.19 -3 -2 0 0.13 0.21 -3 -2 0 0.09 0.25 3 2 0 0.08 0.19 3 2 0 0.09 0.35 3 2 0 0.16 0.17 3 2 0 0.26 0.14 3 2 0 0.18 0.28 3 2 0 0.31 0.26 3 2 0 0.30 0.22 3 2 0 0.12 0.25 3 2 0 0.33 0.40 3 2 0 0.08 0.25 -4 -2 0 100.30 7.00 -4 -2 0 100.68 6.98 -4 -2 0 100.79 6.95 -4 -2 0 99.10 6.99 -4 -2 0 100.55 6.98 -4 -2 0 104.37 6.99 -4 -2 0 103.92 6.91 -4 -2 0 79.90 6.94 4 2 0 91.26 6.98 4 2 0 84.71 7.02 4 2 0 101.07 6.90 4 2 0 94.01 6.97 4 2 0 94.46 6.94 4 2 0 99.07 6.95 4 2 0 100.71 6.97 4 2 0 98.40 7.00 4 2 0 99.73 6.99 4 2 0 98.65 6.91 -5 -2 0 0.09 0.40 -5 -2 0 0.34 0.35 -5 -2 0 0.11 0.28 -5 -2 0 0.48 0.47 -5 -2 0 0.81 0.37 -5 -2 0 -0.04 0.36 -5 -2 0 0.49 0.20 -5 -2 0 0.63 0.41 5 2 0 -0.14 0.41 5 2 0 0.32 0.23 5 2 0 0.13 0.44 5 2 0 -0.49 0.63 5 2 0 0.51 0.43 -6 -2 0 47.99 3.60 -6 -2 0 53.77 3.64 -6 -2 0 49.35 3.60 -6 -2 0 51.91 3.47 -6 -2 0 42.56 3.54 -6 -2 0 51.59 3.53 -6 -2 0 54.38 3.64 -6 -2 0 51.65 3.64 6 2 0 42.55 3.55 6 2 0 42.88 3.66 6 2 0 45.38 3.63 6 2 0 46.72 3.50 -7 -2 0 0.15 0.45 -7 -2 0 0.00 0.34 -7 -2 0 0.14 0.26 -7 -2 0 -0.13 0.50 -7 -2 0 0.09 0.51 -7 -2 0 -0.22 0.43 -7 -2 0 0.11 0.61 7 2 0 0.09 0.57 7 2 0 -0.01 0.53 7 2 0 -0.16 0.53 7 2 0 -0.13 0.29 -8 -2 0 30.69 2.40 -8 -2 0 29.33 2.18 -8 -2 0 27.43 2.27 -8 -2 0 29.28 2.07 -8 -2 0 28.65 2.30 -8 -2 0 25.31 2.28 -8 -2 0 26.76 2.34 8 2 0 29.03 2.26 8 2 0 27.99 2.13 8 2 0 26.24 2.36 8 2 0 29.82 2.41 -9 -2 0 -0.72 0.60 -9 -2 0 -0.45 0.41 -9 -2 0 -0.19 0.55 -9 -2 0 -1.53 0.72 -9 -2 0 -0.51 0.80 -9 -2 0 -0.57 0.75 -9 -2 0 0.54 0.33 9 2 0 0.36 0.71 9 2 0 -0.28 0.95 9 2 0 -1.26 0.67 9 2 0 -0.35 0.68 9 2 0 0.20 0.38 -10 -2 0 152.43 12.23 -10 -2 0 172.46 12.33 -10 -2 0 147.92 12.22 -10 -2 0 161.08 12.11 -10 -2 0 172.48 12.05 -10 -2 0 151.94 12.25 10 2 0 189.18 12.51 10 2 0 182.19 12.37 10 2 0 174.87 12.29 10 2 0 197.96 12.22 10 2 0 167.54 12.11 -11 -2 0 -0.05 0.51 -11 -2 0 -0.53 0.77 -11 -2 0 0.03 0.94 -11 -2 0 -0.09 0.83 -11 -2 0 -1.01 0.74 -11 -2 0 -0.67 0.38 11 2 0 0.74 0.88 11 2 0 -0.06 0.81 11 2 0 1.02 1.16 11 2 0 0.08 1.17 -12 -2 0 69.66 5.56 -12 -2 0 71.90 5.80 -12 -2 0 73.59 5.48 -12 -2 0 73.59 5.78 -12 -2 0 71.75 5.93 -12 -2 0 69.09 5.79 12 2 0 83.66 6.02 12 2 0 92.53 6.08 12 2 0 87.62 5.86 -13 -2 0 -0.78 0.56 -13 -2 0 -0.91 0.87 -13 -2 0 -0.56 0.76 -13 -2 0 -0.24 0.43 -13 -2 0 -1.16 0.89 -13 -2 0 -2.36 1.27 13 2 0 -0.83 0.99 13 2 0 0.58 1.07 13 2 0 0.70 1.03 13 2 0 1.19 0.98 -14 -2 0 -0.63 0.47 -14 -2 0 -0.06 0.83 -14 -2 0 -1.26 0.58 -14 -2 0 -1.02 0.95 -14 -2 0 -1.18 0.96 -14 -2 0 -2.70 1.04 14 2 0 0.81 1.11 14 2 0 0.30 1.15 14 2 0 -0.74 0.99 14 2 0 -0.05 1.04 -15 -2 0 0.35 1.03 -15 -2 0 -2.54 1.55 -15 -2 0 -0.62 0.86 -15 -2 0 -1.82 0.98 -15 -2 0 -1.72 0.58 -15 -2 0 -0.58 0.47 15 2 0 -1.99 1.02 15 2 0 1.16 1.17 15 2 0 -1.13 1.16 15 2 0 0.30 1.11 -16 -2 0 8.92 1.07 -16 -2 0 6.99 1.60 -16 -2 0 9.87 1.44 -16 -2 0 11.64 1.65 -16 -2 0 8.41 2.05 16 2 0 11.07 1.59 16 2 0 12.79 1.83 16 2 0 11.35 1.68 16 2 0 15.22 1.73 -17 -2 0 -2.57 1.72 -17 -2 0 0.27 0.95 -17 -2 0 -0.99 1.24 -17 -2 0 -2.23 1.04 17 2 0 0.50 1.23 17 2 0 0.12 1.26 17 2 0 0.08 1.17 17 2 0 0.62 1.29 -18 -2 0 58.98 5.19 -18 -2 0 56.81 5.01 -18 -2 0 66.18 5.67 -18 -2 0 60.21 5.04 18 2 0 77.02 5.14 18 2 0 65.33 5.32 18 2 0 63.86 5.23 18 2 0 70.63 5.80 -19 -2 0 -2.56 1.95 -19 -2 0 -0.92 1.31 -19 -2 0 -0.31 1.19 -19 -2 0 1.21 1.41 19 2 0 2.24 1.49 19 2 0 1.39 1.36 19 2 0 2.92 1.96 19 2 0 -1.38 1.44 -20 -2 0 23.20 3.14 -20 -2 0 20.00 2.32 -20 -2 0 16.99 2.32 -20 -2 0 17.93 2.33 20 2 0 26.30 2.52 20 2 0 18.52 2.24 20 2 0 21.94 2.94 20 2 0 16.17 2.35 -21 -2 0 -1.51 2.19 -21 -2 0 -0.29 1.49 -21 -2 0 -0.72 1.25 21 2 0 -0.37 1.94 21 2 0 0.49 1.58 21 2 0 -4.53 1.48 21 2 0 3.59 2.14 21 -2 1 2.29 1.67 21 -2 1 2.01 2.05 21 -2 1 -0.19 1.46 21 -2 1 0.86 1.88 -21 2 -1 -0.01 1.28 -21 2 -1 1.61 2.04 -21 2 -1 -0.45 1.19 20 -2 1 1.66 1.87 20 -2 1 1.16 1.17 20 -2 1 0.76 1.32 20 -2 1 -0.31 1.42 -20 2 -1 -0.75 1.23 -20 2 -1 -0.43 1.16 -20 2 -1 0.00 1.98 19 -2 1 0.70 1.19 19 -2 1 0.94 1.50 19 -2 1 0.80 1.68 19 -2 1 0.39 1.78 -19 2 -1 0.42 1.32 -19 2 -1 0.81 1.19 -19 2 -1 -0.91 1.76 -19 2 -1 -1.43 1.10 18 -2 1 29.58 2.80 18 -2 1 24.96 2.78 18 -2 1 30.56 2.85 18 -2 1 20.66 2.93 -18 2 -1 26.45 2.67 -18 2 -1 33.00 3.32 -18 2 -1 26.24 2.67 -18 2 -1 27.06 2.78 17 -2 1 41.85 4.14 17 -2 1 48.64 3.93 17 -2 1 43.86 3.85 -17 2 -1 44.79 3.80 -17 2 -1 42.77 3.65 -17 2 -1 45.13 3.79 -17 2 -1 55.16 4.33 16 -2 1 0.95 0.97 16 -2 1 -0.81 1.38 16 -2 1 1.16 1.19 -16 2 -1 0.12 1.53 -16 2 -1 1.15 1.09 -16 2 -1 2.15 1.14 -16 2 -1 0.73 0.72 -16 2 -1 0.84 0.96 15 -2 1 6.78 1.37 15 -2 1 8.48 1.34 15 -2 1 7.33 1.52 -15 2 -1 8.87 0.86 -15 2 -1 10.96 1.64 -15 2 -1 7.15 1.22 -15 2 -1 10.38 1.58 -15 2 -1 8.44 0.94 -15 2 -1 9.49 1.38 14 -2 1 32.55 2.84 14 -2 1 24.09 2.71 14 -2 1 23.39 2.93 -14 2 -1 33.58 2.73 -14 2 -1 23.45 2.33 -14 2 -1 31.08 2.73 -14 2 -1 30.75 2.59 -14 2 -1 35.95 2.36 -14 2 -1 33.57 3.15 13 -2 1 2.06 1.07 13 -2 1 -0.58 1.08 13 -2 1 0.25 1.11 -13 2 -1 -1.66 1.22 -13 2 -1 1.83 0.41 -13 2 -1 1.18 0.51 -13 2 -1 1.09 1.00 -13 2 -1 0.17 0.78 -13 2 -1 2.07 0.95 12 -2 1 17.49 1.91 12 -2 1 10.48 1.60 12 -2 1 12.63 1.72 -12 2 -1 18.19 2.02 -12 2 -1 16.33 1.74 -12 2 -1 15.36 1.27 -12 2 -1 16.96 1.78 -12 2 -1 21.26 1.45 -12 2 -1 17.70 1.84 11 -2 1 0.45 0.75 11 -2 1 -2.44 0.88 11 -2 1 -0.18 0.68 -11 2 -1 -1.02 1.09 -11 2 -1 -0.10 0.34 -11 2 -1 -1.05 0.60 -11 2 -1 0.05 0.44 -11 2 -1 -0.27 0.78 -11 2 -1 0.01 0.85 10 -2 1 15.53 1.61 10 -2 1 12.10 1.53 -10 2 -1 18.16 1.92 -10 2 -1 14.77 1.20 -10 2 -1 16.45 1.57 -10 2 -1 16.69 1.69 -10 2 -1 18.37 1.62 9 -2 1 0.92 0.59 9 -2 1 0.25 0.78 -9 2 -1 1.27 0.47 -9 2 -1 1.44 0.97 -9 2 -1 1.38 0.57 -9 2 -1 0.64 0.77 -9 2 -1 1.63 0.55 -9 2 -1 1.94 0.41 -9 2 -1 1.80 0.33 8 -2 1 -0.24 0.66 8 -2 1 0.08 0.45 8 -2 1 -0.39 0.47 -8 2 -1 -0.50 0.44 -8 2 -1 -0.08 0.25 -8 2 -1 -1.08 0.65 -8 2 -1 -0.70 0.81 -8 2 -1 0.16 0.37 7 -2 1 12.29 1.25 7 -2 1 13.98 1.38 7 -2 1 13.02 1.19 -7 2 -1 14.54 1.03 -7 2 -1 12.20 1.40 -7 2 -1 13.77 1.39 -7 2 -1 13.05 1.24 -7 2 -1 14.42 1.11 6 -2 1 2.31 0.46 6 -2 1 3.28 0.40 6 -2 1 3.63 0.36 6 -2 1 2.96 0.52 6 -2 1 3.67 0.54 -6 2 -1 3.95 0.74 -6 2 -1 2.39 0.49 -6 2 -1 1.61 0.73 -6 2 -1 3.95 0.34 -6 2 -1 3.95 0.45 -6 2 -1 2.94 0.66 5 -2 1 157.01 10.67 5 -2 1 156.53 10.70 5 -2 1 145.20 10.71 5 -2 1 145.88 10.69 5 -2 1 149.68 10.64 5 -2 1 143.75 10.62 -5 2 -1 145.31 10.76 -5 2 -1 159.57 10.65 -5 2 -1 153.48 10.62 -5 2 -1 151.90 10.65 -5 2 -1 141.97 10.75 -5 2 -1 146.39 10.69 4 -2 1 6.27 0.91 4 -2 1 8.83 0.83 4 -2 1 8.33 0.78 4 -2 1 8.66 0.76 4 -2 1 8.71 0.69 4 -2 1 7.78 0.64 4 -2 1 8.48 1.00 -4 2 -1 9.71 0.85 -4 2 -1 8.52 0.96 -4 2 -1 9.26 0.65 -4 2 -1 9.16 0.82 -4 2 -1 7.82 0.75 -4 2 -1 9.28 0.70 -4 2 -1 6.67 0.91 -4 2 -1 8.05 0.95 -4 2 -1 8.73 0.77 -4 2 -1 8.91 0.71 3 -2 1 172.32 12.46 3 -2 1 172.12 12.44 3 -2 1 185.81 12.53 3 -2 1 151.92 12.50 3 -2 1 171.35 12.47 3 -2 1 180.39 12.50 3 -2 1 171.93 12.43 3 -2 1 172.31 12.46 -3 2 -1 180.37 12.51 -3 2 -1 184.64 12.43 -3 2 -1 186.04 12.47 -3 2 -1 180.70 12.50 -3 2 -1 171.27 12.46 -3 2 -1 173.13 12.47 -3 2 -1 170.83 12.43 -3 2 -1 175.30 12.45 -3 2 -1 182.98 12.45 2 -2 1 7.77 0.62 2 -2 1 9.24 0.69 2 -2 1 5.70 0.51 2 -2 1 7.66 0.70 2 -2 1 6.69 0.57 2 -2 1 6.39 0.58 2 -2 1 5.47 0.53 2 -2 1 6.33 0.55 2 -2 1 5.68 0.53 -2 2 -1 7.52 0.52 -2 2 -1 5.56 0.54 -2 2 -1 5.36 0.59 -2 2 -1 8.03 0.55 -2 2 -1 5.45 0.62 -2 2 -1 7.20 0.57 -2 2 -1 6.79 0.59 -2 2 -1 7.37 0.52 1 -2 1 37.53 2.69 1 -2 1 37.18 2.68 1 -2 1 37.31 2.67 -1 -2 1 39.16 2.81 -2 -2 1 6.81 0.60 -2 -2 1 7.75 0.57 -2 -2 1 7.39 0.59 -2 -2 1 7.42 0.60 -2 -2 1 7.60 0.65 -2 -2 1 5.66 0.57 -2 -2 1 6.69 0.61 -2 -2 1 6.27 0.63 2 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0.07 0.23 0 -3 0 0.34 0.22 0 -3 0 0.41 0.14 0 -3 0 0.31 0.24 0 3 0 0.48 0.25 0 3 0 0.21 0.16 0 3 0 0.03 0.14 0 3 0 0.23 0.20 0 3 0 0.00 0.22 0 3 0 0.29 0.17 0 3 0 0.17 0.24 0 3 0 0.09 0.11 0 3 0 0.42 0.19 0 3 0 0.63 0.20 -1 -3 0 0.36 0.26 -1 -3 0 0.01 0.15 -1 -3 0 0.17 0.21 -1 -3 0 0.17 0.18 -1 -3 0 -0.05 0.12 -1 -3 0 -0.02 0.13 -1 -3 0 0.33 0.18 -1 -3 0 -0.04 0.12 -1 -3 0 -0.02 0.15 -1 -3 0 -0.03 0.16 1 3 0 -0.15 0.18 1 3 0 0.20 0.15 1 3 0 0.15 0.16 1 3 0 -0.14 0.21 1 3 0 -0.04 0.16 1 3 0 0.38 0.17 1 3 0 0.08 0.25 1 3 0 -0.12 0.12 1 3 0 0.18 0.26 1 3 0 -0.16 0.15 -2 -3 0 72.75 5.18 -2 -3 0 71.75 5.17 -2 -3 0 70.02 5.18 -2 -3 0 73.15 5.17 -2 -3 0 76.44 5.16 -2 -3 0 76.29 5.14 -2 -3 0 71.96 5.18 -2 -3 0 67.68 5.18 -2 -3 0 73.13 5.15 -2 -3 0 71.28 5.16 2 3 0 70.49 5.16 2 3 0 72.83 5.15 2 3 0 73.85 5.17 2 3 0 69.42 5.19 2 3 0 76.49 5.14 2 3 0 71.49 5.18 2 3 0 70.59 5.19 2 3 0 69.68 5.17 2 3 0 74.07 5.16 -3 -3 0 0.57 0.30 -3 -3 0 0.21 0.20 -3 -3 0 0.11 0.23 -3 -3 0 0.43 0.24 -3 -3 0 0.41 0.17 -3 -3 0 0.20 0.19 -3 -3 0 0.30 0.27 -3 -3 0 0.79 0.38 3 3 0 0.04 0.27 3 3 0 0.36 0.31 3 3 0 0.40 0.27 3 3 0 0.52 0.23 3 3 0 0.33 0.26 3 3 0 0.31 0.31 3 3 0 0.38 0.20 3 3 0 0.27 0.32 -4 -3 0 8.73 0.70 -4 -3 0 9.24 0.83 -4 -3 0 8.64 0.73 -4 -3 0 8.61 0.85 -4 -3 0 8.36 0.75 -4 -3 0 8.67 0.85 -4 -3 0 8.39 0.71 -4 -3 0 8.63 0.90 4 3 0 8.01 0.88 4 3 0 8.71 0.75 4 3 0 8.27 0.95 4 3 0 8.79 0.82 4 3 0 8.13 0.68 4 3 0 8.69 0.92 -5 -3 0 0.11 0.22 -5 -3 0 0.26 0.36 -5 -3 0 0.37 0.34 -5 -3 0 -0.16 0.33 -5 -3 0 0.58 0.43 -5 -3 0 0.36 0.29 -5 -3 0 0.39 0.40 5 3 0 -0.31 0.54 5 3 0 -0.01 0.20 5 3 0 0.28 0.32 5 3 0 0.11 0.24 5 3 0 0.12 0.44 5 3 0 0.04 0.60 -6 -3 0 33.50 2.48 -6 -3 0 33.91 2.50 -6 -3 0 27.88 2.40 -6 -3 0 34.64 2.49 -6 -3 0 34.56 2.42 -6 -3 0 34.49 2.49 -6 -3 0 32.86 2.34 6 3 0 33.33 2.40 6 3 0 28.10 2.64 6 3 0 28.22 2.64 6 3 0 31.62 2.48 6 3 0 31.98 2.38 -7 -3 0 0.39 0.36 -7 -3 0 0.52 0.46 -7 -3 0 0.31 0.27 -7 -3 0 0.71 0.60 -7 -3 0 0.59 0.53 -7 -3 0 -0.08 0.56 -7 -3 0 0.33 0.51 7 3 0 -0.43 0.44 7 3 0 -0.14 0.15 7 3 0 -0.33 0.71 7 3 0 0.16 0.55 7 3 0 -0.22 0.77 7 3 0 0.30 0.30 -8 -3 0 51.05 3.80 -8 -3 0 51.26 3.55 -8 -3 0 53.65 3.79 -8 -3 0 48.12 3.72 -8 -3 0 50.60 3.65 -8 -3 0 50.84 3.72 -8 -3 0 50.01 3.73 8 3 0 50.84 3.52 8 3 0 44.11 3.72 8 3 0 48.24 3.97 8 3 0 45.02 3.65 8 3 0 46.11 3.93 8 3 0 48.71 3.60 -9 -3 0 0.09 0.67 -9 -3 0 0.30 0.58 -9 -3 0 -0.25 0.30 -9 -3 0 0.23 0.55 -9 -3 0 0.32 0.46 -9 -3 0 -0.42 0.59 -9 -3 0 -0.16 0.66 9 3 0 -0.05 0.70 9 3 0 -0.56 0.25 9 3 0 -0.53 0.70 9 3 0 0.41 0.36 9 3 0 -1.13 0.74 9 3 0 0.32 1.02 -10 -3 0 0.63 0.63 -10 -3 0 0.53 0.72 -10 -3 0 0.77 0.96 -10 -3 0 0.72 0.51 -10 -3 0 0.87 0.38 -10 -3 0 -0.37 0.84 -10 -3 0 0.30 0.65 10 3 0 0.14 0.86 10 3 0 0.48 0.78 10 3 0 0.69 0.40 10 3 0 1.13 1.11 10 3 0 0.45 0.31 10 3 0 0.90 0.83 -11 -3 0 -1.03 0.91 -11 -3 0 -0.13 0.53 -11 -3 0 0.20 0.65 -11 -3 0 -0.15 0.38 -11 -3 0 -0.87 0.81 -11 -3 0 -0.67 1.05 -11 -3 0 -1.12 0.90 11 3 0 -0.68 0.81 11 3 0 -0.28 0.88 11 3 0 -0.05 0.46 11 3 0 0.95 0.91 11 3 0 -0.58 0.83 -12 -3 0 9.89 1.49 -12 -3 0 9.42 1.42 -12 -3 0 11.93 1.40 -12 -3 0 12.35 1.59 -12 -3 0 11.86 1.05 -12 -3 0 11.00 1.15 12 3 0 11.24 1.05 12 3 0 15.24 1.89 12 3 0 12.44 1.50 12 3 0 13.71 1.90 12 3 0 13.06 1.26 12 3 0 17.12 1.55 -13 -3 0 -0.90 0.58 -13 -3 0 -0.89 0.89 -13 -3 0 -0.99 1.09 -13 -3 0 -0.77 0.92 -13 -3 0 -3.69 1.29 -13 -3 0 -0.23 0.44 13 3 0 -1.40 0.99 13 3 0 -0.50 1.37 13 3 0 0.65 1.40 13 3 0 -0.37 0.45 13 3 0 -1.32 1.00 -14 -3 0 -0.07 1.19 -14 -3 0 -0.35 1.09 -14 -3 0 0.22 0.61 -14 -3 0 -1.13 1.14 -14 -3 0 0.04 0.45 -14 -3 0 -0.75 1.18 14 3 0 2.27 1.20 14 3 0 1.22 1.16 14 3 0 -0.75 1.04 14 3 0 -0.45 1.07 -15 -3 0 -1.16 0.44 -15 -3 0 -2.71 1.17 -15 -3 0 -0.97 1.05 -15 -3 0 0.58 0.93 -15 -3 0 -3.59 1.52 -15 -3 0 -1.18 0.61 15 3 0 -0.30 1.13 15 3 0 -1.21 1.08 15 3 0 0.89 1.31 15 3 0 0.54 1.19 -16 -3 0 14.67 1.95 -16 -3 0 17.65 2.06 -16 -3 0 18.26 1.66 -16 -3 0 16.31 1.88 -16 -3 0 14.71 1.67 -16 -3 0 15.13 2.43 16 3 0 16.77 2.35 16 3 0 17.05 2.09 16 3 0 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17.16 1.45 2 -5 4 16.58 1.36 2 -5 4 16.58 1.29 2 -5 4 16.96 1.29 2 -5 4 16.80 1.24 -2 5 -4 17.38 1.41 -2 5 -4 16.33 1.41 -2 5 -4 15.14 1.35 -2 5 -4 16.89 1.40 -2 5 -4 16.77 1.33 -2 5 -4 17.02 1.42 1 -5 4 133.27 9.70 1 -5 4 134.13 9.64 1 -5 4 128.59 9.70 1 -5 4 135.21 9.73 1 -5 4 138.29 9.75 1 -5 4 142.84 9.71 -1 5 -4 135.19 9.74 -1 5 -4 134.08 9.73 -1 5 -4 144.40 9.72 -1 5 -4 126.19 9.74 -1 5 -4 141.33 9.78 -1 5 -4 139.52 9.73 0 -5 4 0.49 0.32 0 -5 4 0.39 0.39 0 -5 4 0.06 0.21 0 -5 4 -0.01 0.30 0 -5 4 -0.21 0.38 0 -5 4 -0.17 0.38 0 -5 4 0.17 0.40 0 5 -4 -0.33 0.36 0 5 -4 0.21 0.36 0 5 -4 -0.60 0.48 0 5 -4 0.11 0.09 0 5 -4 -0.03 0.38 0 5 -4 0.24 0.42 0 5 -4 -0.02 0.39 -1 -5 4 131.09 9.73 -1 -5 4 138.59 9.70 -1 -5 4 141.47 9.72 -1 -5 4 137.87 9.78 -1 -5 4 137.08 9.76 -1 -5 4 142.78 9.79 1 5 -4 131.04 9.76 1 5 -4 137.24 9.76 1 5 -4 135.40 9.78 1 5 -4 136.50 9.77 1 5 -4 133.69 9.68 1 5 -4 137.12 9.68 1 5 -4 133.74 9.76 1 5 -4 135.82 9.70 -2 -5 4 17.56 1.29 -2 -5 4 16.30 1.41 -2 -5 4 17.83 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0.84 -6 -5 4 5.63 0.84 -6 -5 4 6.41 0.57 -6 -5 4 4.65 0.84 -6 -5 4 5.79 0.67 -6 -5 4 5.82 0.77 -6 -5 4 6.95 0.74 6 5 -4 5.53 0.71 6 5 -4 6.14 0.99 6 5 -4 4.94 0.70 6 5 -4 6.35 0.58 6 5 -4 5.76 0.74 6 5 -4 5.71 0.81 -7 -5 4 43.91 3.89 -7 -5 4 50.41 3.56 -7 -5 4 51.16 3.69 -7 -5 4 50.60 3.84 -7 -5 4 44.28 3.87 -7 -5 4 52.36 3.68 -7 -5 4 50.95 3.78 7 5 -4 49.32 3.75 7 5 -4 49.22 3.59 7 5 -4 47.59 3.73 7 5 -4 51.82 3.84 7 5 -4 50.85 3.74 7 5 -4 51.20 3.83 -8 -5 4 23.80 2.11 -8 -5 4 23.10 1.87 -8 -5 4 18.83 2.35 -8 -5 4 23.84 1.86 -8 -5 4 19.30 2.02 -8 -5 4 24.15 2.08 8 5 -4 22.33 2.16 8 5 -4 24.88 2.15 8 5 -4 21.91 1.93 8 5 -4 24.34 1.98 8 5 -4 23.86 2.13 -9 -5 4 28.49 2.59 -9 -5 4 31.01 2.43 -9 -5 4 25.52 2.70 -9 -5 4 28.00 2.60 -9 -5 4 25.18 2.85 -9 -5 4 32.48 2.36 9 5 -4 32.66 2.71 9 5 -4 28.21 2.42 9 5 -4 32.78 2.50 9 5 -4 32.93 2.70 -10 -5 4 -1.03 0.78 -10 -5 4 -0.64 0.75 -10 -5 4 -0.16 0.51 -10 -5 4 -1.50 1.05 -10 -5 4 -0.77 0.68 -10 -5 4 -0.60 1.02 10 5 -4 0.13 0.78 10 5 -4 0.33 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-2 3.01 1.22 0 22 2 0.77 1.41 0 22 2 0.65 1.40 0 22 2 0.73 1.79 0 22 2 3.57 1.50 -1 -22 -2 0.30 1.09 -1 -22 -2 3.16 1.58 -1 -22 -2 0.81 1.54 1 22 2 -0.10 1.19 1 22 2 0.71 1.41 1 22 2 1.32 1.11 -2 -22 -2 1.70 1.61 -2 -22 -2 1.47 1.11 -2 -22 -2 4.77 1.68 2 22 2 1.48 1.37 2 22 2 1.78 1.43 2 22 2 0.52 1.39 -3 -22 -2 5.54 1.81 -3 -22 -2 7.65 1.47 -3 -22 -2 7.72 1.80 3 22 2 5.81 1.53 3 22 2 5.51 1.39 3 22 2 7.26 1.61 3 -22 -1 0.20 1.44 3 -22 -1 1.07 1.15 -3 22 1 1.77 1.53 -3 22 1 2.64 1.05 -3 22 1 1.90 1.50 -3 22 1 1.10 1.35 2 -22 -1 2.61 1.53 2 -22 -1 2.05 1.18 -2 22 1 2.33 1.50 -2 22 1 4.68 1.46 -2 22 1 1.53 1.17 -2 22 1 -0.18 1.79 1 -22 -1 2.60 1.18 1 -22 -1 1.18 1.13 1 -22 -1 1.75 1.50 -1 22 1 1.52 1.30 -1 22 1 1.58 1.13 -1 22 1 0.51 1.81 -1 22 1 2.74 1.13 0 -22 -1 47.73 3.97 0 -22 -1 43.17 3.57 0 -22 -1 41.62 3.90 0 22 1 49.05 4.46 0 22 1 44.28 4.31 0 22 1 47.14 3.84 0 22 1 45.92 3.86 0 22 1 42.04 3.64 -1 -22 -1 2.22 1.61 -1 -22 -1 3.67 1.59 -1 -22 -1 2.90 1.08 1 22 1 1.53 1.46 1 22 1 1.38 1.32 1 22 1 1.88 1.42 1 22 1 2.00 1.17 -2 -22 -1 1.32 1.53 -2 -22 -1 3.17 1.64 -2 -22 -1 0.24 1.04 2 22 1 1.73 1.44 2 22 1 0.00 1.26 2 22 1 0.53 1.19 -3 -22 -1 1.79 1.61 -3 -22 -1 -0.49 1.07 -3 -22 -1 2.48 1.66 3 22 1 0.75 1.22 3 22 1 -0.44 1.40 3 22 1 0.63 1.29 3 -22 0 2.12 2.54 3 -22 0 -0.48 1.46 3 -22 0 0.03 1.05 -3 22 0 0.60 1.13 -3 22 0 -0.52 1.28 -3 22 0 2.09 1.37 -3 22 0 -1.08 1.82 2 -22 0 8.61 1.78 2 -22 0 12.36 1.87 -2 22 0 9.61 1.59 -2 22 0 10.16 1.75 -2 22 0 9.31 2.19 -2 22 0 10.39 1.80 1 -22 0 1.37 1.46 1 -22 0 0.21 1.45 -1 22 0 0.60 1.44 -1 22 0 -0.72 1.20 -1 22 0 -0.91 1.19 -1 22 0 0.95 1.58 -1 22 0 0.78 1.84 0 -22 0 16.14 1.81 0 -22 0 14.08 2.07 0 -22 0 11.46 1.64 0 22 0 11.67 2.37 0 22 0 14.94 1.76 0 22 0 14.98 1.99 0 22 0 14.58 1.83 -1 -22 0 0.28 1.13 -1 -22 0 1.28 1.52 -1 -22 0 0.03 1.48 1 22 0 0.65 1.43 1 22 0 -0.08 1.32 1 22 0 -0.15 1.04 1 22 0 -1.20 1.84 -2 -22 0 9.22 1.40 -2 -22 0 10.95 1.63 -2 -22 0 11.33 1.94 2 22 0 10.77 2.32 2 22 0 10.92 1.79 2 22 0 11.18 1.76 2 22 0 10.29 1.58 -3 -22 0 -0.14 1.16 -3 -22 0 -1.40 1.02 -3 -22 0 0.62 1.14 3 22 0 0.39 1.40 3 22 0 -0.90 1.22 3 22 0 -0.01 1.24 3 -22 1 2.37 1.47 3 -22 1 1.66 1.44 3 -22 1 2.65 1.61 -3 22 -1 -0.39 1.80 -3 22 -1 0.46 1.45 2 -22 1 1.99 1.46 2 -22 1 3.27 1.50 -2 22 -1 0.40 1.25 -2 22 -1 2.57 1.52 -2 22 -1 2.68 1.90 1 -22 1 1.85 1.52 1 -22 1 3.65 1.54 -1 22 -1 2.58 1.92 -1 22 -1 2.70 1.49 -1 22 -1 1.98 1.32 0 -22 1 44.18 3.92 0 -22 1 47.05 3.97 0 22 -1 42.44 3.74 0 22 -1 47.02 3.90 0 22 -1 46.45 4.38 -1 -22 1 1.33 1.32 -1 -22 1 3.77 1.23 -1 -22 1 2.31 1.57 1 22 -1 2.74 1.48 1 22 -1 1.38 1.23 1 22 -1 0.57 1.92 -2 -22 1 0.97 1.14 -2 -22 1 2.28 1.01 -2 -22 1 1.51 1.20 2 22 -1 1.02 1.94 2 22 -1 0.77 1.23 2 22 -1 2.04 1.46 -3 -22 1 1.10 1.02 -3 -22 1 1.79 1.60 -3 -22 1 0.02 1.16 3 22 -1 0.68 1.44 3 22 -1 -0.80 1.36 3 22 -1 1.52 1.30 3 -22 2 7.84 1.71 3 -22 2 7.69 1.64 3 -22 2 11.31 1.75 -3 22 -2 6.94 1.70 -3 22 -2 7.94 1.77 -3 22 -2 6.80 1.46 2 -22 2 0.74 1.09 2 -22 2 2.46 1.16 2 -22 2 3.98 1.38 -2 22 -2 2.83 1.53 -2 22 -2 1.40 1.31 -2 22 -2 2.81 1.49 1 -22 2 0.80 1.12 1 -22 2 0.25 1.47 -1 22 -2 0.83 1.34 -1 22 -2 2.52 1.49 -1 22 -2 -0.13 1.41 0 -22 2 4.12 1.55 0 -22 2 1.78 1.15 0 22 -2 1.93 1.23 0 22 -2 2.98 1.49 0 22 -2 -0.24 1.85 -1 -22 2 3.67 1.56 -1 -22 2 0.95 1.49 1 22 -2 2.50 1.47 1 22 -2 0.39 1.40 1 22 -2 -0.54 1.87 -2 -22 2 3.16 1.61 -2 -22 2 3.12 1.58 2 22 -2 1.52 1.97 2 22 -2 2.92 1.34 2 22 -2 4.49 1.53 -3 -22 2 5.40 1.75 -3 -22 2 5.63 1.15 -3 -22 2 6.20 1.68 3 22 -2 7.44 1.81 3 22 -2 5.97 1.49 3 22 -2 7.25 1.62 2 -22 3 6.65 1.66 2 -22 3 5.85 1.57 2 -22 3 4.01 1.26 -2 22 -3 6.19 1.63 -2 22 -3 4.53 1.59 -2 22 -3 5.84 1.35 1 -22 3 21.47 2.43 1 -22 3 20.22 2.20 -1 22 -3 18.69 2.51 -1 22 -3 25.29 2.55 -1 22 -3 22.15 2.38 0 -22 3 6.65 1.34 0 -22 3 3.15 1.22 0 22 -3 6.47 2.05 0 22 -3 5.99 1.42 0 22 -3 6.15 1.61 -1 -22 3 21.86 2.51 -1 -22 3 24.70 2.50 1 22 -3 19.03 2.30 1 22 -3 24.78 2.56 1 22 -3 24.26 3.00 -2 -22 3 7.28 1.72 -2 -22 3 7.13 1.77 2 22 -3 3.99 2.10 2 22 -3 4.87 1.43 2 22 -3 3.50 1.52 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 9064 _shelx_res_file ; TITL 1a in Pbca CELL 0.71073 18.01950 18.74180 19.74010 90.0000 90.0000 90.0000 ZERR 8.00 0.00100 0.00100 0.00120 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H BR MN N DISP $C 0.00341 0.00169 11.32113!source kissel DISP $H -0.00002 0.00000 0.66638!source kissel DISP $Br -0.27128 2.47050 10018.37566!source kissel DISP $Mn 0.33931 0.73667 3000.91578!source kissel DISP $N 0.00664 0.00342 19.38436!source kissel UNIT 240 368 32 8 32 OMIT 2 1 0 OMIT 0 2 0 OMIT 1 0 2 OMIT 1 1 1 OMIT 2 0 0 OMIT 0 0 2 OMIT 1 2 1 OMIT 0 2 2 OMIT 2 1 1 ACTA 50 TEMP -150 SIZE 0.05 0.22 0.22 L.S. 20 BOND $H HTAB C1 Br2 EQIV $1 -x+1, y+1/2, -z+1/2 HTAB C2 Br1_$1 EQIV $2 -x+1/2, y+1/2, z HTAB C3 Br4_$2 HTAB C5 Br4_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C13 Br2_$3 HTAB C16 Br2 HTAB C16 Br4 EQIV $4 x-1/2, -y+1/2, -z+1 HTAB C17 Br1_$4 EQIV $5 x, -y+1/2, z+1/2 HTAB C18 Br3_$5 HTAB C19 Br1_$5 HTAB C22 Br4 HTAB C28 Br1_$4 LIST 4 FMAP 2 PLAN 10 WGHT 0.023700 8.992200 FVAR 0.04183 MN1 4 0.400859 0.310171 0.385648 11.00000 0.01755 0.01621 = 0.01559 -0.00331 0.00031 -0.00057 BR1 3 0.499231 0.265191 0.306154 11.00000 0.02003 0.02671 = 0.01650 -0.00284 0.00028 0.00503 BR2 3 0.452157 0.370289 0.489754 11.00000 0.02955 0.02120 = 0.01475 -0.00201 -0.00276 -0.00469 BR3 3 0.326595 0.401846 0.322988 11.00000 0.02716 0.02358 = 0.02490 -0.00604 -0.00927 0.00703 BR4 3 0.324638 0.207999 0.427674 11.00000 0.02775 0.02007 = 0.03297 -0.00875 0.01042 -0.00772 N1 5 0.362617 0.576103 0.406083 11.00000 0.01992 0.01700 = 0.02146 -0.00183 0.00423 -0.00276 C1 1 0.424101 0.540315 0.391337 11.00000 0.02160 0.01344 = 0.01755 -0.00121 0.00027 -0.00017 AFIX 43 H1 2 0.439346 0.496947 0.412002 11.00000 -1.20000 AFIX 0 N2 5 0.460738 0.574610 0.343335 11.00000 0.02099 0.01359 = 0.01623 0.00013 0.00148 0.00007 C2 1 0.420845 0.635430 0.327288 11.00000 0.03047 0.01889 = 0.02613 0.00583 0.00518 0.00458 AFIX 43 H2 2 0.434195 0.670310 0.294564 11.00000 -1.20000 AFIX 0 C3 1 0.359846 0.636177 0.366374 11.00000 0.02897 0.02101 = 0.03059 0.00289 0.00489 0.00839 AFIX 43 H3 2 0.322035 0.671501 0.366516 11.00000 -1.20000 AFIX 0 C4 1 0.307199 0.552524 0.455962 11.00000 0.02480 0.02084 = 0.03158 0.00102 0.00990 -0.00336 AFIX 23 H4A 2 0.314928 0.501263 0.465799 11.00000 -1.20000 H4B 2 0.256969 0.558028 0.436328 11.00000 -1.20000 AFIX 0 C5 1 0.311488 0.594035 0.521005 11.00000 0.02236 0.03242 = 0.02205 0.00648 0.00168 -0.00109 AFIX 137 H5A 2 0.362796 0.594196 0.537468 11.00000 -1.50000 H5B 2 0.279274 0.571767 0.554960 11.00000 -1.50000 H5C 2 0.295191 0.643202 0.512991 11.00000 -1.50000 AFIX 0 C6 1 0.529873 0.549791 0.309457 11.00000 0.02071 0.01457 = 0.01544 -0.00040 0.00180 0.00089 C7 1 0.556946 0.481066 0.343336 11.00000 0.02511 0.01606 = 0.01482 0.00225 -0.00007 0.00081 AFIX 23 H7A 2 0.566827 0.489967 0.391940 11.00000 -1.20000 H7B 2 0.518222 0.443776 0.339843 11.00000 -1.20000 AFIX 0 C8 1 0.627845 0.455739 0.308460 11.00000 0.02199 0.01890 = 0.01947 0.00029 0.00078 0.00323 AFIX 13 H8 2 0.645599 0.410944 0.330704 11.00000 -1.20000 AFIX 0 C9 1 0.611310 0.440685 0.233665 11.00000 0.02609 0.02045 = 0.02021 -0.00565 0.00350 0.00210 AFIX 23 H9A 2 0.656870 0.423860 0.210633 11.00000 -1.20000 H9B 2 0.573123 0.402920 0.229859 11.00000 -1.20000 AFIX 0 C10 1 0.583514 0.509235 0.200073 11.00000 0.03334 0.02652 = 0.01271 -0.00120 0.00079 0.00513 AFIX 13 H10 2 0.572778 0.499746 0.151195 11.00000 -1.20000 AFIX 0 C11 1 0.643829 0.566882 0.205742 11.00000 0.03474 0.02690 = 0.02368 0.00622 0.01239 0.00407 AFIX 23 H11A 2 0.689467 0.550680 0.182440 11.00000 -1.20000 H11B 2 0.626647 0.611311 0.183609 11.00000 -1.20000 AFIX 0 C12 1 0.660630 0.581375 0.280498 11.00000 0.02444 0.02232 = 0.02784 -0.00127 0.00777 -0.00482 AFIX 13 H12 2 0.699859 0.618915 0.284197 11.00000 -1.20000 AFIX 0 C13 1 0.589485 0.607301 0.315393 11.00000 0.02582 0.01525 = 0.02072 -0.00085 0.00167 -0.00606 AFIX 23 H13A 2 0.599629 0.617412 0.363739 11.00000 -1.20000 H13B 2 0.572015 0.651888 0.293739 11.00000 -1.20000 AFIX 0 C14 1 0.513336 0.535310 0.234854 11.00000 0.02858 0.02311 = 0.01553 -0.00048 -0.00327 0.00397 AFIX 23 H14A 2 0.473912 0.498755 0.230905 11.00000 -1.20000 H14B 2 0.495597 0.579558 0.212760 11.00000 -1.20000 AFIX 0 C15 1 0.687653 0.512796 0.314172 11.00000 0.02119 0.03195 = 0.02299 -0.00070 0.00128 0.00088 AFIX 23 H15A 2 0.733671 0.496138 0.291801 11.00000 -1.20000 H15B 2 0.698906 0.521976 0.362481 11.00000 -1.20000 AFIX 0 N3 5 0.318850 0.232558 0.641211 11.00000 0.01777 0.01996 = 0.01875 0.00059 -0.00229 0.00353 C16 1 0.294124 0.275626 0.593284 11.00000 0.01691 0.01758 = 0.01639 -0.00218 -0.00052 -0.00117 AFIX 43 H16 2 0.322663 0.293831 0.556697 11.00000 -1.20000 AFIX 0 N4 5 0.222929 0.289325 0.604560 11.00000 0.01583 0.02027 = 0.01682 0.00135 0.00051 0.00110 C17 1 0.201824 0.253113 0.662224 11.00000 0.01960 0.03006 = 0.02276 0.01207 0.00273 0.00239 AFIX 43 H17 2 0.153826 0.253154 0.682133 11.00000 -1.20000 AFIX 0 C18 1 0.261513 0.217849 0.685006 11.00000 0.02709 0.02665 = 0.01932 0.00658 0.00221 0.00160 AFIX 43 H18 2 0.263784 0.188276 0.724037 11.00000 -1.20000 AFIX 0 C19 1 0.393193 0.200640 0.644095 11.00000 0.01963 0.02698 = 0.02483 -0.00320 -0.00753 0.00619 AFIX 23 H19A 2 0.413737 0.206540 0.690270 11.00000 -1.20000 H19B 2 0.426354 0.225868 0.612076 11.00000 -1.20000 AFIX 0 C20 1 0.391128 0.122767 0.626466 11.00000 0.03153 0.02775 = 0.04255 -0.00442 0.00282 0.01034 AFIX 137 H20A 2 0.374643 0.117050 0.579469 11.00000 -1.50000 H20B 2 0.356532 0.098082 0.656765 11.00000 -1.50000 H20C 2 0.440860 0.102322 0.631653 11.00000 -1.50000 AFIX 0 C21 1 0.172066 0.331874 0.560992 11.00000 0.01293 0.01745 = 0.01505 0.00211 -0.00049 0.00256 C22 1 0.215386 0.368288 0.504401 11.00000 0.01701 0.02023 = 0.01782 0.00181 0.00535 0.00284 AFIX 23 H22A 2 0.241624 0.332045 0.476878 11.00000 -1.20000 H22B 2 0.252822 0.400976 0.524001 11.00000 -1.20000 AFIX 0 C23 1 0.161379 0.410361 0.459618 11.00000 0.02496 0.01778 = 0.01720 0.00569 0.00349 0.00238 AFIX 13 H23 2 0.189548 0.434166 0.422279 11.00000 -1.20000 AFIX 0 C24 1 0.122292 0.466900 0.502417 11.00000 0.02674 0.01641 = 0.02697 0.00399 0.00265 0.00419 AFIX 23 H24A 2 0.159388 0.500110 0.521765 11.00000 -1.20000 H24B 2 0.087838 0.494767 0.473677 11.00000 -1.20000 AFIX 0 C25 1 0.079224 0.430711 0.559438 11.00000 0.02252 0.02039 = 0.02412 0.00197 0.00681 0.00768 AFIX 13 H25 2 0.053535 0.467779 0.587328 11.00000 -1.20000 AFIX 0 C26 1 0.021797 0.379803 0.529657 11.00000 0.01958 0.03083 = 0.02861 0.01093 -0.00130 0.00575 AFIX 23 H26A 2 -0.013940 0.406847 0.501521 11.00000 -1.20000 H26B 2 -0.006050 0.356322 0.566698 11.00000 -1.20000 AFIX 0 C27 1 0.060575 0.323332 0.486285 11.00000 0.02361 0.02494 = 0.02658 0.00426 -0.00855 -0.00436 AFIX 13 H27 2 0.022755 0.290264 0.466569 11.00000 -1.20000 AFIX 0 C28 1 0.114920 0.280946 0.530323 11.00000 0.02252 0.01626 = 0.02076 0.00314 -0.00128 -0.00140 AFIX 23 H28A 2 0.087561 0.256204 0.566924 11.00000 -1.20000 H28B 2 0.140381 0.244490 0.502448 11.00000 -1.20000 AFIX 0 C29 1 0.103996 0.359314 0.429184 11.00000 0.03369 0.02248 = 0.01746 0.00221 -0.00402 0.00437 AFIX 23 H29A 2 0.069543 0.386091 0.399523 11.00000 -1.20000 H29B 2 0.129344 0.322702 0.401409 11.00000 -1.20000 AFIX 0 C30 1 0.132620 0.388169 0.604449 11.00000 0.02218 0.02034 = 0.01692 0.00019 0.00465 0.00169 AFIX 23 H30A 2 0.104721 0.364597 0.641405 11.00000 -1.20000 H30B 2 0.169613 0.420660 0.625023 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1a in Pbca REM R1 = 0.0269 for 5029 Fo > 4sig(Fo) and 0.0410 for all 5883 data REM 354 parameters refined using 0 restraints END WGHT 0.0236 9.0298 REM Highest difference peak 0.716, deepest hole -0.504, 1-sigma level 0.091 Q1 1 0.3153 0.2216 0.3887 11.00000 0.05 0.72 Q2 1 0.5004 0.2187 0.3124 11.00000 0.05 0.46 Q3 1 0.4987 0.3029 0.3287 11.00000 0.05 0.40 Q4 1 0.4385 0.3571 0.4465 11.00000 0.05 0.39 Q5 1 0.3866 0.2438 0.4229 11.00000 0.05 0.37 Q6 1 0.3263 0.4108 0.2770 11.00000 0.05 0.37 Q7 1 0.1144 0.4126 0.5766 11.00000 0.05 0.37 Q8 1 0.4979 0.2937 0.2680 11.00000 0.05 0.37 Q9 1 0.5177 0.5431 0.2732 11.00000 0.05 0.36 Q10 1 0.4598 0.4020 0.5381 11.00000 0.05 0.35 ; _shelx_res_checksum 56136 _shelxl_version_number 201.4 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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 Mn Mn1 0.40086(3) 0.31017(2) 0.38565(2) 0.01650(10) Uani d 1 . . Br Br1 0.49923(2) 0.26519(2) 0.30615(2) 0.02108(8) Uani d 1 . . Br Br2 0.45216(2) 0.37029(2) 0.48975(2) 0.02183(9) Uani d 1 . . Br Br3 0.32660(2) 0.40185(2) 0.32299(2) 0.02521(9) Uani d 1 . . Br Br4 0.32464(2) 0.20800(2) 0.42767(2) 0.02693(9) Uani d 1 . . N N1 0.3626(2) 0.57610(10) 0.40610(10) 0.0195(6) Uani d 1 . . C C1 0.4241(2) 0.5403(2) 0.3913(2) 0.0175(7) Uani d 1 . . H H1 0.4393 0.4969 0.4120 0.021 Uiso calc 1 . . N N2 0.46070(10) 0.57460(10) 0.34330(10) 0.0169(6) Uani d 1 . . C C2 0.4208(2) 0.6354(2) 0.3273(2) 0.0252(8) Uani d 1 . . H H2 0.4342 0.6703 0.2946 0.030 Uiso calc 1 . . C C3 0.3598(2) 0.6362(2) 0.3664(2) 0.0269(8) Uani d 1 . . H H3 0.3220 0.6715 0.3665 0.032 Uiso calc 1 . . C C4 0.3072(2) 0.5525(2) 0.4560(2) 0.0257(8) Uani d 1 . . H H4A 0.3149 0.5013 0.4658 0.031 Uiso calc 1 . . H H4B 0.2570 0.5580 0.4363 0.031 Uiso calc 1 . . C C5 0.3115(2) 0.5940(2) 0.5210(2) 0.0256(8) Uani d 1 . . H H5A 0.3628 0.5942 0.5375 0.038 Uiso calc 1 . . H H5B 0.2793 0.5718 0.5550 0.038 Uiso calc 1 . . H H5C 0.2952 0.6432 0.5130 0.038 Uiso calc 1 . . C C6 0.5299(2) 0.5498(2) 0.3095(2) 0.0169(7) Uani d 1 . . C C7 0.5569(2) 0.4811(2) 0.3433(2) 0.0187(7) Uani d 1 . . H H7A 0.5668 0.4900 0.3919 0.022 Uiso calc 1 . . H H7B 0.5182 0.4438 0.3398 0.022 Uiso calc 1 . . C C8 0.6278(2) 0.4557(2) 0.3085(2) 0.0201(7) Uani d 1 . . H H8 0.6456 0.4109 0.3307 0.024 Uiso calc 1 . . C C9 0.6113(2) 0.4407(2) 0.2337(2) 0.0223(7) Uani d 1 . . H H9A 0.6569 0.4239 0.2106 0.027 Uiso calc 1 . . H H9B 0.5731 0.4029 0.2299 0.027 Uiso calc 1 . . C C10 0.5835(2) 0.5092(2) 0.2001(2) 0.0242(8) Uani d 1 . . H H10 0.5728 0.4997 0.1512 0.029 Uiso calc 1 . . C C11 0.6438(2) 0.5669(2) 0.2057(2) 0.0284(8) Uani d 1 . . H H11A 0.6895 0.5507 0.1824 0.034 Uiso calc 1 . . H H11B 0.6266 0.6113 0.1836 0.034 Uiso calc 1 . . C C12 0.6606(2) 0.5814(2) 0.2805(2) 0.0249(8) Uani d 1 . . H H12 0.6999 0.6189 0.2842 0.030 Uiso calc 1 . . C C13 0.5895(2) 0.6073(2) 0.3154(2) 0.0206(7) Uani d 1 . . H H13A 0.5996 0.6174 0.3637 0.025 Uiso calc 1 . . H H13B 0.5720 0.6519 0.2937 0.025 Uiso calc 1 . . C C14 0.5133(2) 0.5353(2) 0.2349(2) 0.0224(7) Uani d 1 . . H H14A 0.4739 0.4988 0.2309 0.027 Uiso calc 1 . . H H14B 0.4956 0.5796 0.2128 0.027 Uiso calc 1 . . C C15 0.6877(2) 0.5128(2) 0.3142(2) 0.0254(8) Uani d 1 . . H H15A 0.7337 0.4961 0.2918 0.030 Uiso calc 1 . . H H15B 0.6989 0.5220 0.3625 0.030 Uiso calc 1 . . N N3 0.31890(10) 0.23260(10) 0.64120(10) 0.0188(6) Uani d 1 . . C C16 0.2941(2) 0.2756(2) 0.5933(2) 0.0170(7) Uani d 1 . . H H16 0.3227 0.2938 0.5567 0.020 Uiso calc 1 . . N N4 0.22290(10) 0.28930(10) 0.60460(10) 0.0176(6) Uani d 1 . . C C17 0.2018(2) 0.2531(2) 0.6622(2) 0.0241(7) Uani d 1 . . H H17 0.1538 0.2532 0.6821 0.029 Uiso calc 1 . . C C18 0.2615(2) 0.2178(2) 0.6850(2) 0.0244(8) Uani d 1 . . H H18 0.2638 0.1883 0.7240 0.029 Uiso calc 1 . . C C19 0.3932(2) 0.2006(2) 0.6441(2) 0.0238(7) Uani d 1 . . H H19A 0.4137 0.2065 0.6903 0.029 Uiso calc 1 . . H H19B 0.4264 0.2259 0.6121 0.029 Uiso calc 1 . . C C20 0.3911(2) 0.1228(2) 0.6265(2) 0.0339(9) Uani d 1 . . H H20A 0.3746 0.1171 0.5795 0.051 Uiso calc 1 . . H H20B 0.3565 0.0981 0.6568 0.051 Uiso calc 1 . . H H20C 0.4409 0.1023 0.6317 0.051 Uiso calc 1 . . C C21 0.1721(2) 0.3319(2) 0.5610(2) 0.0151(6) Uani d 1 . . C C22 0.2154(2) 0.3683(2) 0.5044(2) 0.0184(7) Uani d 1 . . H H22A 0.2416 0.3320 0.4769 0.022 Uiso calc 1 . . H H22B 0.2528 0.4010 0.5240 0.022 Uiso calc 1 . . C C23 0.1614(2) 0.4104(2) 0.4596(2) 0.0200(7) Uani d 1 . . H H23 0.1895 0.4342 0.4223 0.024 Uiso calc 1 . . C C24 0.1223(2) 0.4669(2) 0.5024(2) 0.0234(7) Uani d 1 . . H H24A 0.1594 0.5001 0.5218 0.028 Uiso calc 1 . . H H24B 0.0878 0.4948 0.4737 0.028 Uiso calc 1 . . C C25 0.0792(2) 0.4307(2) 0.5594(2) 0.0223(7) Uani d 1 . . H H25 0.0535 0.4678 0.5873 0.027 Uiso calc 1 . . C C26 0.0218(2) 0.3798(2) 0.5297(2) 0.0263(8) Uani d 1 . . H H26A -0.0139 0.4068 0.5015 0.032 Uiso calc 1 . . H H26B -0.0061 0.3563 0.5667 0.032 Uiso calc 1 . . C C27 0.0606(2) 0.3233(2) 0.4863(2) 0.0250(7) Uani d 1 . . H H27 0.0228 0.2903 0.4666 0.030 Uiso calc 1 . . C C28 0.1149(2) 0.2810(2) 0.5303(2) 0.0198(7) Uani d 1 . . H H28A 0.0876 0.2562 0.5669 0.024 Uiso calc 1 . . H H28B 0.1404 0.2445 0.5024 0.024 Uiso calc 1 . . C C29 0.1040(2) 0.3593(2) 0.4292(2) 0.0245(8) Uani d 1 . . H H29A 0.0695 0.3861 0.3995 0.029 Uiso calc 1 . . H H29B 0.1293 0.3227 0.4014 0.029 Uiso calc 1 . . C C30 0.1326(2) 0.3882(2) 0.6044(2) 0.0198(7) Uani d 1 . . H H30A 0.1047 0.3646 0.6414 0.024 Uiso calc 1 . . H H30B 0.1696 0.4207 0.6250 0.024 Uiso calc 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 Mn1 0.0176(3) 0.0162(2) 0.0156(2) -0.0006(2) 0.0003(2) -0.0033(2) Br1 0.0200(2) 0.0267(2) 0.0165(2) 0.00500(10) 0.00030(10) -0.00280(10) Br2 0.0295(2) 0.0212(2) 0.0148(2) -0.00470(10) -0.00280(10) -0.00200(10) Br3 0.0272(2) 0.0236(2) 0.0249(2) 0.00700(10) -0.00930(10) -0.00600(10) Br4 0.0278(2) 0.0201(2) 0.0330(2) -0.00770(10) 0.0104(2) -0.00880(10) N1 0.020(2) 0.0170(10) 0.0220(10) -0.0030(10) 0.0040(10) -0.0020(10) C1 0.022(2) 0.013(2) 0.018(2) 0.0000(10) 0.0000(10) -0.0010(10) N2 0.0210(10) 0.0140(10) 0.0160(10) 0.0000(10) 0.0020(10) 0.0000(10) C2 0.030(2) 0.019(2) 0.026(2) 0.0050(10) 0.005(2) 0.0060(10) C3 0.029(2) 0.021(2) 0.031(2) 0.008(2) 0.005(2) 0.003(2) C4 0.025(2) 0.021(2) 0.032(2) -0.0030(10) 0.010(2) 0.0010(10) C5 0.022(2) 0.032(2) 0.022(2) -0.001(2) 0.0020(10) 0.007(2) C6 0.021(2) 0.015(2) 0.015(2) 0.0010(10) 0.0020(10) 0.0000(10) C7 0.025(2) 0.016(2) 0.015(2) 0.0010(10) 0.0000(10) 0.0020(10) C8 0.022(2) 0.019(2) 0.020(2) 0.0030(10) 0.0010(10) 0.0000(10) C9 0.026(2) 0.021(2) 0.020(2) 0.0020(10) 0.0040(10) -0.0060(10) C10 0.033(2) 0.026(2) 0.013(2) 0.005(2) 0.0010(10) -0.0010(10) C11 0.035(2) 0.027(2) 0.024(2) 0.004(2) 0.012(2) 0.006(2) C12 0.024(2) 0.022(2) 0.028(2) -0.0050(10) 0.008(2) -0.0010(10) C13 0.026(2) 0.015(2) 0.021(2) -0.0060(10) 0.0020(10) -0.0010(10) C14 0.029(2) 0.023(2) 0.015(2) 0.0040(10) -0.0030(10) -0.0010(10) C15 0.021(2) 0.032(2) 0.023(2) 0.001(2) 0.0010(10) -0.0010(10) N3 0.0180(10) 0.0200(10) 0.0190(10) 0.0040(10) -0.0020(10) 0.0010(10) C16 0.017(2) 0.018(2) 0.016(2) -0.0010(10) -0.0010(10) -0.0020(10) N4 0.0160(10) 0.0200(10) 0.0170(10) 0.0010(10) 0.0010(10) 0.0010(10) C17 0.020(2) 0.030(2) 0.023(2) 0.002(2) 0.0030(10) 0.0120(10) C18 0.027(2) 0.027(2) 0.019(2) 0.002(2) 0.002(2) 0.0070(10) C19 0.020(2) 0.027(2) 0.025(2) 0.0060(10) -0.0070(10) -0.0030(10) C20 0.032(2) 0.028(2) 0.043(2) 0.010(2) 0.003(2) -0.004(2) C21 0.013(2) 0.017(2) 0.015(2) 0.0030(10) -0.0010(10) 0.0020(10) C22 0.017(2) 0.020(2) 0.018(2) 0.0030(10) 0.0050(10) 0.0020(10) C23 0.025(2) 0.018(2) 0.017(2) 0.0020(10) 0.0040(10) 0.0060(10) C24 0.027(2) 0.016(2) 0.027(2) 0.0040(10) 0.003(2) 0.0040(10) C25 0.023(2) 0.020(2) 0.024(2) 0.0080(10) 0.0070(10) 0.0020(10) C26 0.020(2) 0.031(2) 0.029(2) 0.006(2) -0.001(2) 0.011(2) C27 0.024(2) 0.025(2) 0.027(2) -0.004(2) -0.009(2) 0.0040(10) C28 0.023(2) 0.016(2) 0.021(2) -0.0010(10) -0.0010(10) 0.0030(10) C29 0.034(2) 0.023(2) 0.018(2) 0.004(2) -0.004(2) 0.0020(10) C30 0.022(2) 0.020(2) 0.017(2) 0.0020(10) 0.0050(10) 0.0000(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0034 0.0017 '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' Br Br -0.2713 2.4705 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3393 0.7367 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0066 0.0034 '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 Br4 Mn1 Br3 . . 113.33(2) Br4 Mn1 Br1 . . 109.76(2) Br3 Mn1 Br1 . . 107.37(2) Br4 Mn1 Br2 . . 105.88(2) Br3 Mn1 Br2 . . 106.98(2) Br1 Mn1 Br2 . . 113.61(2) C1 N1 C3 . . 108.6(3) C1 N1 C4 . . 124.2(3) C3 N1 C4 . . 127.2(3) N2 C1 N1 . . 109.2(3) N2 C1 H1 . . 125.4 N1 C1 H1 . . 125.4 C1 N2 C2 . . 107.8(3) C1 N2 C6 . . 126.0(3) C2 N2 C6 . . 126.1(3) C3 C2 N2 . . 107.6(3) C3 C2 H2 . . 126.2 N2 C2 H2 . . 126.2 C2 C3 N1 . . 106.8(3) C2 C3 H3 . . 126.6 N1 C3 H3 . . 126.6 N1 C4 C5 . . 112.4(3) N1 C4 H4A . . 109.1 C5 C4 H4A . . 109.1 N1 C4 H4B . . 109.1 C5 C4 H4B . . 109.1 H4A C4 H4B . . 107.9 C4 C5 H5A . . 109.5 C4 C5 H5B . . 109.5 H5A C5 H5B . . 109.5 C4 C5 H5C . . 109.5 H5A C5 H5C . . 109.5 H5B C5 H5C . . 109.5 N2 C6 C13 . . 109.5(2) N2 C6 C14 . . 109.0(3) C13 C6 C14 . . 109.7(3) N2 C6 C7 . . 109.5(2) C13 C6 C7 . . 109.7(3) C14 C6 C7 . . 109.5(2) C8 C7 C6 . . 109.3(2) C8 C7 H7A . . 109.8 C6 C7 H7A . . 109.8 C8 C7 H7B . . 109.8 C6 C7 H7B . . 109.8 H7A C7 H7B . . 108.3 C15 C8 C7 . . 109.9(3) C15 C8 C9 . . 109.8(3) C7 C8 C9 . . 109.2(3) C15 C8 H8 . . 109.3 C7 C8 H8 . . 109.3 C9 C8 H8 . . 109.3 C10 C9 C8 . . 109.1(3) C10 C9 H9A . . 109.9 C8 C9 H9A . . 109.9 C10 C9 H9B . . 109.9 C8 C9 H9B . . 109.9 H9A C9 H9B . . 108.3 C14 C10 C9 . . 110.3(3) C14 C10 C11 . . 109.2(3) C9 C10 C11 . . 109.1(3) C14 C10 H10 . . 109.4 C9 C10 H10 . . 109.4 C11 C10 H10 . . 109.4 C12 C11 C10 . . 109.6(3) C12 C11 H11A . . 109.8 C10 C11 H11A . . 109.8 C12 C11 H11B . . 109.8 C10 C11 H11B . . 109.8 H11A C11 H11B . . 108.2 C15 C12 C11 . . 109.5(3) C15 C12 C13 . . 109.7(3) C11 C12 C13 . . 108.9(3) C15 C12 H12 . . 109.6 C11 C12 H12 . . 109.6 C13 C12 H12 . . 109.6 C6 C13 C12 . . 109.3(3) C6 C13 H13A . . 109.8 C12 C13 H13A . . 109.8 C6 C13 H13B . . 109.8 C12 C13 H13B . . 109.8 H13A C13 H13B . . 108.3 C10 C14 C6 . . 109.3(3) C10 C14 H14A . . 109.8 C6 C14 H14A . . 109.8 C10 C14 H14B . . 109.8 C6 C14 H14B . . 109.8 H14A C14 H14B . . 108.3 C8 C15 C12 . . 109.5(3) C8 C15 H15A . . 109.8 C12 C15 H15A . . 109.8 C8 C15 H15B . . 109.8 C12 C15 H15B . . 109.8 H15A C15 H15B . . 108.2 C16 N3 C18 . . 108.6(3) C16 N3 C19 . . 125.8(3) C18 N3 C19 . . 125.4(3) N3 C16 N4 . . 108.9(3) N3 C16 H16 . . 125.5 N4 C16 H16 . . 125.5 C16 N4 C17 . . 108.1(3) C16 N4 C21 . . 127.0(3) C17 N4 C21 . . 124.8(3) C18 C17 N4 . . 107.4(3) C18 C17 H17 . . 126.3 N4 C17 H17 . . 126.3 C17 C18 N3 . . 107.0(3) C17 C18 H18 . . 126.5 N3 C18 H18 . . 126.5 N3 C19 C20 . . 111.4(3) N3 C19 H19A . . 109.4 C20 C19 H19A . . 109.4 N3 C19 H19B . . 109.4 C20 C19 H19B . . 109.4 H19A C19 H19B . . 108.0 C19 C20 H20A . . 109.5 C19 C20 H20B . . 109.5 H20A C20 H20B . . 109.5 C19 C20 H20C . . 109.5 H20A C20 H20C . . 109.5 H20B C20 H20C . . 109.5 N4 C21 C22 . . 110.4(2) N4 C21 C28 . . 108.0(2) C22 C21 C28 . . 109.5(2) N4 C21 C30 . . 109.3(2) C22 C21 C30 . . 109.8(2) C28 C21 C30 . . 109.8(3) C21 C22 C23 . . 109.1(3) C21 C22 H22A . . 109.9 C23 C22 H22A . . 109.9 C21 C22 H22B . . 109.9 C23 C22 H22B . . 109.9 H22A C22 H22B . . 108.3 C24 C23 C29 . . 109.8(3) C24 C23 C22 . . 109.3(3) C29 C23 C22 . . 109.5(3) C24 C23 H23 . . 109.4 C29 C23 H23 . . 109.4 C22 C23 H23 . . 109.4 C25 C24 C23 . . 109.5(3) C25 C24 H24A . . 109.8 C23 C24 H24A . . 109.8 C25 C24 H24B . . 109.8 C23 C24 H24B . . 109.8 H24A C24 H24B . . 108.2 C26 C25 C24 . . 109.8(3) C26 C25 C30 . . 108.9(3) C24 C25 C30 . . 109.8(3) C26 C25 H25 . . 109.4 C24 C25 H25 . . 109.4 C30 C25 H25 . . 109.4 C25 C26 C27 . . 109.8(3) C25 C26 H26A . . 109.7 C27 C26 H26A . . 109.7 C25 C26 H26B . . 109.7 C27 C26 H26B . . 109.7 H26A C26 H26B . . 108.2 C29 C27 C26 . . 109.9(3) C29 C27 C28 . . 108.7(3) C26 C27 C28 . . 109.5(3) C29 C27 H27 . . 109.6 C26 C27 H27 . . 109.6 C28 C27 H27 . . 109.6 C21 C28 C27 . . 109.4(2) C21 C28 H28A . . 109.8 C27 C28 H28A . . 109.8 C21 C28 H28B . . 109.8 C27 C28 H28B . . 109.8 H28A C28 H28B . . 108.2 C27 C29 C23 . . 109.4(3) C27 C29 H29A . . 109.8 C23 C29 H29A . . 109.8 C27 C29 H29B . . 109.8 C23 C29 H29B . . 109.8 H29A C29 H29B . . 108.2 C25 C30 C21 . . 108.9(2) C25 C30 H30A . . 109.9 C21 C30 H30A . . 109.9 C25 C30 H30B . . 109.9 C21 C30 H30B . . 109.9 H30A C30 H30B . . 108.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 Br4 . 2.4983(6) Mn1 Br3 . 2.5046(6) Mn1 Br1 . 2.5130(6) Mn1 Br2 . 2.5194(5) N1 C1 . 1.327(4) N1 C3 . 1.373(4) N1 C4 . 1.470(4) C1 N2 . 1.322(4) C1 H1 . 0.9500 N2 C2 . 1.384(4) N2 C6 . 1.488(4) C2 C3 . 1.343(5) C2 H2 . 0.9500 C3 H3 . 0.9500 C4 C5 . 1.503(5) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 H5A . 0.9800 C5 H5B . 0.9800 C5 H5C . 0.9800 C6 C13 . 1.526(4) C6 C14 . 1.527(4) C6 C7 . 1.531(4) C7 C8 . 1.527(4) C7 H7A . 0.9900 C7 H7B . 0.9900 C8 C15 . 1.522(5) C8 C9 . 1.532(4) C8 H8 . 1.0000 C9 C10 . 1.530(4) C9 H9A . 0.9900 C9 H9B . 0.9900 C10 C14 . 1.520(5) C10 C11 . 1.537(5) C10 H10 . 1.0000 C11 C12 . 1.531(5) C11 H11A . 0.9900 C11 H11B . 0.9900 C12 C15 . 1.527(5) C12 C13 . 1.534(5) C12 H12 . 1.0000 C13 H13A . 0.9900 C13 H13B . 0.9900 C14 H14A . 0.9900 C14 H14B . 0.9900 C15 H15A . 0.9900 C15 H15B . 0.9900 N3 C16 . 1.321(4) N3 C18 . 1.375(4) N3 C19 . 1.468(4) C16 N4 . 1.327(4) C16 H16 . 0.9500 N4 C17 . 1.379(4) N4 C21 . 1.488(4) C17 C18 . 1.340(5) C17 H17 . 0.9500 C18 H18 . 0.9500 C19 C20 . 1.501(5) C19 H19A . 0.9900 C19 H19B . 0.9900 C20 H20A . 0.9800 C20 H20B . 0.9800 C20 H20C . 0.9800 C21 C22 . 1.524(4) C21 C28 . 1.529(4) C21 C30 . 1.534(4) C22 C23 . 1.533(4) C22 H22A . 0.9900 C22 H22B . 0.9900 C23 C24 . 1.527(4) C23 C29 . 1.531(5) C23 H23 . 1.0000 C24 C25 . 1.526(4) C24 H24A . 0.9900 C24 H24B . 0.9900 C25 C26 . 1.525(5) C25 C30 . 1.533(4) C25 H25 . 1.0000 C26 C27 . 1.530(5) C26 H26A . 0.9900 C26 H26B . 0.9900 C27 C29 . 1.529(5) C27 C28 . 1.532(4) C27 H27 . 1.0000 C28 H28A . 0.9900 C28 H28B . 0.9900 C29 H29A . 0.9900 C29 H29B . 0.9900 C30 H30A . 0.9900 C30 H30B . 0.9900 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 C1 H1 Br2 . 0.95 2.84 3.766(3) 166.4 C2 H2 Br1 3_655 0.95 2.92 3.864(3) 169.9 C3 H3 Br4 8_665 0.95 2.99 3.785(3) 142.7 C5 H5C Br4 8_665 0.98 3.00 3.738(3) 133.5 C13 H13A Br2 5_666 0.99 3.05 3.941(3) 150.8 C16 H16 Br2 . 0.95 3.04 3.929(3) 156.2 C16 H16 Br4 . 0.95 3.01 3.549(3) 117.2 C17 H17 Br1 4_456 0.95 2.82 3.719(3) 159.1 C18 H18 Br3 7_566 0.95 2.82 3.718(3) 158.2 C19 H19A Br1 7_566 0.99 2.81 3.781(3) 167.5 C22 H22A Br4 . 0.99 2.93 3.898(3) 166.0 C28 H28A Br1 4_456 0.99 3.00 3.939(3) 159.7 _cod_database_fobs_code 1557436