#------------------------------------------------------------------------------ #$Date: 2025-04-05 14:45:22 +0300 (Sat, 05 Apr 2025) $ #$Revision: 299192 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/30/07/2300756.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_2300756 loop_ _publ_author_name 'Biehler, Erik' 'Pagola, Silvina' 'Stam, Daniel' 'Merkelbach, Johannes' 'Jandl, Christian' 'Abdel-Fattah, Tarek M' _publ_section_title ; A comparison of microcrystal electron diffraction and X-ray powder diffraction for the structural analysis of metal-organic frameworks. ; _journal_coeditor_code TE5145SUP1 _journal_issue 'Pt 2' _journal_name_full 'Journal of applied crystallography' _journal_page_first 398 _journal_page_last 411 _journal_paper_doi 10.1107/S1600576724012068 _journal_volume 58 _journal_year 2025 _chemical_compound_source 'synthesized from aqueous solution' _chemical_formula_moiety 'C8 H8 Mn O6' _chemical_formula_sum 'C8 H8 Mn O6' _chemical_formula_weight 255.08 _chemical_name_common 'manganese terephthalate dihydrate' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary XD _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 99.270(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.71(8) _cell_length_b 6.57(3) _cell_length_c 7.37(3) _cell_measurement_reflns_used 1202 _cell_measurement_temperature 293 _cell_measurement_theta_max 1.1655 _cell_measurement_theta_min 0.2537 _cell_volume 894(7) _computing_cell_refinement 'SAINT (Bruker 2019)' _computing_data_collection 'Eldix (ELDICO 2022)' _computing_data_reduction 'SAINT (Bruker 2019)' _computing_molecular_graphics 'Mercury (Macrae 2008)' _computing_publication_material 'EnCIFer (Allen 2004), PLATON (Spek 2009)' _computing_structure_refinement 'SHELXL (Sheldrick 2015), ShelXle (Huebschle 2011)' _computing_structure_solution 'SHELXD (Sheldrick 2008)' _diffrn_ambient_temperature 293 _diffrn_detector 'Dectris QUADRO' _diffrn_detector_area_resol_mean 13.33 _diffrn_measured_fraction_theta_full 0.869 _diffrn_measured_fraction_theta_max 0.765 _diffrn_measurement_device 'ELDICO ED-1' _diffrn_measurement_device_type 'electron diffractometer' _diffrn_measurement_method 'continuous rotation 3D ED' _diffrn_radiation_source LaB~6~ _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.02851 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_unetI/netI 0.0759 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3031 _diffrn_reflns_reduction_process ; ; _diffrn_reflns_theta_full 0.98 _diffrn_reflns_theta_max 1.17 _diffrn_reflns_theta_min 0.13 _exptl_absorpt_coefficient_mu 0 _exptl_absorpt_correction_T_max 0.7431 _exptl_absorpt_correction_T_min 0.2672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2016/2 (Bruker 2016)' _exptl_crystal_colour cream _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description shard _exptl_crystal_F_000 0 _exptl_crystal_size_max 0.005 _exptl_crystal_size_mid 0.001 _exptl_crystal_size_min 0.0002 _refine_diff_density_max 0.223 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef 6139(70) _refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^ _refine_ls_extinction_method 'shelxl-2019/1 (sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 77 _refine_ls_number_reflns 1049 _refine_ls_number_restraints 75 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.1970 _refine_ls_R_factor_gt 0.1817 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'W=1/[\S^2^(FO^2^)+(0.1949P)^2^+3.1104P] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4498 _refine_ls_wR_factor_ref 0.4608 _reflns_number_gt 893 _reflns_number_total 1049 _reflns_threshold_expression I>2\s(I) _cod_data_source_file te5145.cif _cod_data_source_block III _cod_depositor_comments 'Adding full bibliography for 2300754--2300756.cif.' _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2300756 _shelx_res_file ; REM Best SHELXD solution FINAL CC 81.44 REM Fragments: 8 REM TITL Mn_tereph_merger in C2/c Mn_tereph_merger.res created by SHELXL-2018/3 at 16:34:50 on 02-Mar-2023 CELL 0.02851 18.71080 6.57010 7.37020 90.0000 99.2695 90.0000 ZERR 4.00000 0.08090 0.02840 0.03180 0.0000 0.0126 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C 0.1361 0.3731 0.5482 3.2814 1.2266 13.0456 0.5971 41.0202 0 = 0 0 0 0.77 12.01 SFAC H 0.0367 0.5608 0.1269 3.7913 0.236 13.5557 0.129 37.7229 0 0 = 0 0 0.32 1.008 SFAC Mn 0.5552 0.3947 2.0073 3.48 2.5678 19.5862 2.3695 74.9201 0 0 = 0 0 1.37 54.94 SFAC O 0.1433 0.3055 0.5103 2.2683 0.937 8.2625 0.3923 25.6645 0 0 = 0 0 0.66 16 REM source: REM for neutral atoms: REM Electron atomic scattering factors and scattering potentials of crystals REM L.-M. Peng, Micron 30 (1999) 625?648. REM for ions: REM International Tables for Crystallography Vol C Table 4.3.1.2 REM (gnuplot fit of Cromer-Mann parameters inspired by Tim Gruene)) UNIT 32 32 4 24 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 10 BOND $H PLAN 20 ACTA HTAB RIGU SIMU FMAP 2 TEMP 20 WGHT 0.194900 3.110400 EXTI 6138.708496 FVAR 1.35228 MN01 3 0.250000 0.250000 0.000000 10.50000 0.02031 0.02377 = 0.02054 -0.00131 -0.00397 0.00286 O1 4 0.182800 0.340987 0.201772 11.00000 0.03148 0.02514 = 0.03055 -0.00184 -0.00277 -0.00070 C1 1 0.033597 0.683736 0.057831 11.00000 0.01302 0.01563 = 0.05217 -0.00704 -0.01225 -0.00305 AFIX 43 H1B 2 0.056588 0.805853 0.094685 11.00000 -1.20000 AFIX 0 O2 4 0.170387 0.668150 0.267838 11.00000 0.02376 0.02796 = 0.03352 -0.00119 -0.01655 -0.00514 C2 1 0.068331 0.500975 0.093498 11.00000 0.02202 0.01694 = 0.02695 -0.00134 -0.00540 -0.00006 O3 4 0.194390 -0.045219 -0.016975 11.00000 0.03877 0.02294 = 0.03603 0.00372 -0.00720 -0.00685 H1 2 0.192210 -0.133616 -0.114873 11.00000 -1.50000 H1A 2 0.182150 -0.119889 0.086086 11.00000 -1.50000 C3 1 0.037682 0.319688 0.035989 11.00000 0.01935 0.01537 = 0.04255 -0.00210 -0.01464 0.00258 AFIX 43 H3 2 0.063765 0.199359 0.058710 11.00000 -1.20000 AFIX 0 C4 1 0.145748 0.503358 0.196388 11.00000 0.01571 0.02441 = 0.02439 -0.00524 -0.00450 -0.00508 HKLF 4 REM Mn_tereph_merger in C2/c REM wR2 = 0.4608, GooF = S = 1.054, Restrained GooF = 1.019 for all data REM R1 = 0.1817 for 893 Fo > 4sig(Fo) and 0.1970 for all 1049 data REM 77 parameters refined using 75 restraints END WGHT 0.1739 2.3115 REM Instructions for potential hydrogen bonds EQIV $6 x, -y, z-1/2 HTAB O3 O1_$6 EQIV $7 x, y-1, z HTAB O3 O2_$7 REM Highest difference peak 0.223, deepest hole -0.251, 1-sigma level 0.065 Q1 1 0.1930 0.6481 0.1818 11.00000 0.05 0.22 Q2 1 0.1967 0.0664 -0.0359 11.00000 0.05 0.21 Q3 1 0.1987 0.0238 0.1023 11.00000 0.05 0.21 Q4 1 0.2061 0.3327 0.1834 11.00000 0.05 0.20 Q5 1 0.2266 0.2413 0.1850 11.00000 0.05 0.19 Q6 1 0.1630 -0.0026 0.1588 11.00000 0.05 0.19 Q7 1 0.0762 0.7699 0.2870 11.00000 0.05 0.18 Q8 1 0.2478 0.4824 0.2037 11.00000 0.05 0.18 Q9 1 0.0796 0.1860 -0.1020 11.00000 0.05 0.17 Q10 1 0.0919 0.8334 0.1290 11.00000 0.05 0.17 Q11 1 0.0474 0.0276 0.0390 11.00000 0.05 0.17 Q12 1 0.1623 -0.3028 0.0701 11.00000 0.05 0.17 Q13 1 0.0403 0.6711 0.2894 11.00000 0.05 0.17 Q14 1 0.1334 0.1664 0.0565 11.00000 0.05 0.16 Q15 1 0.1206 0.4673 0.2399 11.00000 0.05 0.16 Q16 1 0.1524 0.5647 0.2395 11.00000 0.05 0.16 Q17 1 0.0822 0.8328 0.0230 11.00000 0.05 0.15 Q18 1 0.0876 0.8732 0.0018 11.00000 0.05 0.15 Q19 1 0.1251 -0.1636 0.1459 11.00000 0.05 0.15 Q20 1 0.0694 0.1742 0.1882 11.00000 0.05 0.14 ; _shelx_res_checksum 3335 _shelx_hkl_file ; -1 -1 0 220.17 18.05 1 -1 0 245.77 17.97 1 1 0 266.60 18.08 -1 1 0 247.12 17.96 -3 -1 0 18.97 3.26 3 -1 0 16.64 2.35 -3 1 0 17.20 2.34 3 1 0 19.58 3.26 -5 -1 0 142.55 11.49 5 1 0 145.62 11.48 -7 -1 0 154.12 13.11 7 1 0 159.91 13.23 0 -2 0 177.74 12.60 0 -2 0 155.15 12.16 0 2 0 166.06 12.16 -2 -2 0 192.28 14.83 2 -2 0 219.05 14.68 2 2 0 199.45 14.85 2 2 0 178.83 14.60 4 -2 0 496.70 40.42 -4 2 0 599.23 40.50 4 2 0 555.35 40.70 -6 -2 0 56.54 6.03 6 -2 0 55.31 5.18 6 2 0 58.91 5.90 -6 2 0 52.94 5.20 8 -2 0 130.81 11.12 -8 2 0 143.99 11.11 8 2 0 113.32 10.44 -10 -2 0 147.68 12.44 -12 -2 0 38.63 6.16 12 2 0 37.82 6.26 -14 -2 0 309.25 25.65 1 -3 0 90.76 6.55 -1 3 0 83.69 6.56 3 -3 0 90.71 7.11 -3 -3 0 90.31 7.02 5 -3 0 926.90 68.17 -5 -3 0 828.79 68.16 5 -3 0 966.07 68.44 -5 3 0 1000.00 68.23 7 -3 0 11.81 2.16 -7 -3 0 15.43 3.56 7 3 0 15.20 3.37 -7 3 0 16.27 2.38 9 -3 0 77.33 6.95 -9 -3 0 87.54 7.73 9 3 0 79.51 6.60 9 3 0 64.29 7.39 -9 3 0 73.61 6.98 -11 -3 0 63.18 6.23 11 -3 0 74.15 7.27 -11 3 0 62.60 6.96 13 -3 0 385.04 28.91 -13 3 0 342.83 28.78 13 3 0 360.89 28.23 -15 -3 0 229.37 18.94 15 -3 0 210.42 19.58 15 3 0 229.08 18.74 -17 -3 0 22.66 5.96 17 3 0 14.58 4.36 -19 -3 0 7.22 5.04 -21 -3 0 -0.35 4.36 0 -4 0 173.72 13.69 0 -4 0 200.08 14.46 2 -4 0 49.81 4.89 4 -4 0 53.32 4.22 -4 -4 0 39.30 3.99 -4 4 0 47.65 4.14 6 -4 0 264.39 20.25 -6 -4 0 257.12 20.54 6 -4 0 264.38 20.58 -6 4 0 275.66 20.34 6 4 0 288.82 20.43 -8 -4 0 98.40 8.64 8 -4 0 115.22 9.52 8 -4 0 100.38 8.70 -8 4 0 122.42 8.88 8 4 0 107.93 9.43 8 4 0 99.51 8.58 -10 -4 0 136.31 12.25 -10 -4 0 162.80 13.40 10 -4 0 162.56 12.68 -10 4 0 165.38 12.74 10 4 0 167.49 13.47 12 -4 0 50.12 5.39 -12 -4 0 42.61 4.75 12 4 0 45.67 4.82 -12 4 0 52.73 5.70 12 4 0 44.25 6.20 -14 -4 0 28.15 5.70 -14 -4 0 32.56 4.30 -14 4 0 38.72 5.48 14 4 0 44.12 4.60 -16 -4 0 15.49 3.81 16 4 0 8.00 2.76 -18 -4 0 28.97 5.17 -18 4 0 26.80 6.19 -20 -4 0 19.99 5.51 1 -5 0 336.71 24.21 1 -5 0 333.18 25.32 -1 -5 0 302.95 24.16 -1 5 0 356.48 25.55 1 5 0 322.27 24.17 -3 -5 0 5.71 1.84 3 5 0 3.01 1.63 -3 5 0 3.11 1.04 3 5 0 5.54 1.25 5 -5 0 41.19 3.73 -5 -5 0 34.43 3.46 -5 5 0 34.52 3.57 7 -5 0 7.86 1.64 -7 -5 0 9.33 2.63 7 -5 0 6.70 2.01 -7 -5 0 9.33 2.77 -7 5 0 5.90 1.59 -7 5 0 5.97 1.87 7 5 0 10.28 2.69 9 -5 0 91.53 8.96 9 5 0 101.18 9.12 -9 5 0 108.82 9.10 -11 -5 0 12.32 3.96 11 -5 0 15.96 2.41 11 5 0 12.73 3.87 -11 5 0 11.99 2.63 -13 -5 0 3.57 2.90 -13 -5 0 3.69 1.85 13 5 0 7.07 2.71 -13 5 0 5.46 2.21 -15 -5 0 14.75 4.58 -15 5 0 11.46 3.33 -17 -5 0 11.82 3.97 -17 5 0 15.47 4.13 19 5 0 0.01 1.39 -19 5 0 0.91 2.68 0 -6 0 398.65 27.53 0 -6 0 324.33 26.36 2 -6 0 110.42 7.56 2 -6 0 91.72 8.94 -2 -6 0 91.21 7.45 -2 6 0 96.26 9.06 2 6 0 97.21 7.50 2 6 0 108.09 8.35 -2 6 0 92.74 7.54 -4 -6 0 52.61 4.42 -4 6 0 51.70 4.33 4 6 0 51.33 4.41 -6 -6 0 94.04 7.82 -6 -6 0 82.25 8.48 -6 6 0 102.06 7.90 6 6 0 107.88 7.96 6 6 0 108.85 8.62 -6 6 0 88.80 7.95 -8 -6 0 177.73 13.75 8 -6 0 186.87 13.95 -8 6 0 159.06 13.65 8 6 0 172.25 13.96 8 6 0 174.65 13.85 -10 -6 0 47.09 5.40 -10 -6 0 52.12 4.91 10 6 0 44.19 4.62 -10 6 0 36.41 4.68 -10 6 0 44.80 4.54 -12 -6 0 11.68 2.69 12 -6 0 9.50 3.11 -14 -6 0 8.87 2.56 -14 -6 0 5.99 2.99 -14 6 0 9.82 2.63 -16 -6 0 11.98 2.79 -16 -6 0 11.94 4.05 -16 6 0 15.09 3.18 -18 -6 0 3.99 3.20 -18 6 0 1.95 2.23 -20 -6 0 25.88 5.56 1 -7 0 25.34 2.03 -1 -7 0 25.84 2.04 -1 7 0 24.79 3.59 -1 7 0 19.88 1.97 1 7 0 21.29 3.02 1 7 0 19.34 2.01 3 -7 0 36.73 3.08 3 7 0 32.52 3.06 -3 7 0 33.73 2.98 5 -7 0 4.77 1.34 5 7 0 5.86 1.20 5 7 0 5.98 1.89 7 -7 0 17.84 2.76 -7 -7 0 17.70 2.40 -7 7 0 23.69 2.76 -9 -7 0 10.55 2.29 9 -7 0 6.39 2.24 11 -7 0 6.46 2.38 -11 7 0 8.79 2.17 11 7 0 9.94 2.66 13 -7 0 5.97 2.52 -13 -7 0 5.07 2.68 -13 7 0 4.02 1.67 -15 -7 0 9.11 3.24 -15 7 0 5.68 1.95 -17 -7 0 3.21 2.69 0 8 0 2.58 1.64 2 -8 0 20.64 1.98 -2 -8 0 18.99 1.80 -2 8 0 16.36 3.39 4 8 0 6.14 2.19 -4 8 0 7.67 2.59 6 -8 0 20.93 2.39 -6 -8 0 18.86 2.29 6 8 0 21.87 3.07 -8 -8 0 22.01 2.72 8 -8 0 18.78 2.86 -8 8 0 27.91 3.10 8 8 0 23.22 3.52 10 -8 0 6.50 2.10 -10 -8 0 6.78 2.19 -12 -8 0 18.50 3.44 -12 8 0 22.50 3.02 -1 -9 0 1.77 0.62 1 -9 0 1.53 0.55 -1 9 0 0.56 1.58 1 9 0 1.10 1.33 -3 -9 0 1.92 0.65 3 -9 0 3.44 1.01 3 9 0 2.46 1.43 -3 9 0 4.25 2.25 -5 -9 0 7.00 1.32 5 -9 0 5.21 1.28 -5 9 0 9.13 2.63 5 9 0 4.31 1.95 7 -9 0 1.89 1.02 -7 -9 0 2.83 1.05 7 9 0 1.60 1.58 -7 9 0 3.13 1.63 4 0 -1 5.25 2.67 -4 0 1 1.82 2.13 -4 0 1 6.94 3.55 -2 0 1 5.15 1.90 2 0 -1 6.51 1.51 -2 0 1 7.89 1.33 0 0 1 5.99 1.29 0 0 -1 9.67 1.31 -2 0 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2.05 2 -2 1 94.56 7.06 2 -2 1 96.22 7.22 -2 2 -1 84.86 7.17 4 -2 1 70.41 5.90 4 -2 1 81.43 6.29 -4 2 -1 77.29 5.96 -4 2 -1 67.60 6.17 6 -2 1 40.34 3.95 6 -2 1 35.56 4.87 -6 2 -1 43.45 4.05 8 -2 1 10.73 2.92 -8 -2 -1 12.41 3.16 8 2 1 10.17 3.08 -8 2 -1 8.42 2.84 10 -2 1 2.43 2.36 -10 2 -1 3.55 2.69 12 -2 1 -1.14 3.05 -12 2 -1 2.01 3.09 -21 -3 1 10.32 5.93 -17 -3 1 44.82 7.00 17 3 -1 46.13 6.95 -15 -3 1 33.80 5.81 -15 -3 1 26.67 5.74 15 3 -1 37.18 5.86 -13 -3 1 24.97 5.48 -13 -3 1 19.41 4.12 13 3 -1 17.38 4.03 13 3 -1 11.74 4.19 -11 -3 1 29.32 3.74 11 -3 -1 24.62 5.06 11 3 -1 17.26 4.51 11 3 -1 21.91 3.50 7 -3 -1 37.46 4.03 -7 -3 1 44.10 4.64 -7 3 1 41.70 4.16 5 -3 -1 152.82 11.31 -5 -3 1 153.53 11.37 -5 -3 1 124.82 11.48 5 3 -1 149.93 11.62 -5 3 1 153.67 11.32 5 3 -1 149.03 11.39 3 -3 -1 229.07 16.96 3 -3 -1 206.79 17.02 -3 3 1 253.63 16.98 3 3 -1 245.45 17.53 -3 3 1 207.84 16.98 -1 -3 1 359.40 27.39 -1 -3 1 352.53 26.95 1 -3 -1 361.36 26.87 1 3 -1 385.24 27.41 1 3 -1 381.86 26.96 -1 -3 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2.04 0.84 2 -2 -8 -0.06 0.90 -2 -2 8 1.44 0.73 2 2 -8 1.34 1.28 -2 2 8 2.55 1.10 2 2 -8 -0.08 1.11 0 -2 8 8.58 1.36 0 2 -8 4.66 2.03 -2 -2 -8 58.77 5.00 2 2 8 69.10 5.34 4 -2 8 4.59 1.50 -4 2 -8 8.56 2.06 -6 -2 -8 12.35 2.12 6 2 8 17.21 2.62 -8 -2 -8 10.40 2.74 -8 2 -8 15.78 2.17 8 2 8 13.52 2.74 -10 -2 -8 14.30 3.75 -10 2 -8 11.16 2.31 12 2 8 23.89 4.18 -12 2 -8 21.54 3.27 17 -3 -8 0.01 1.57 -17 3 8 3.42 2.58 -15 3 8 6.75 2.32 13 3 -8 7.18 2.44 -13 3 8 -0.33 3.91 -11 -3 8 10.62 2.34 -11 3 8 10.68 2.06 11 3 -8 10.43 2.89 -11 3 8 9.67 4.50 9 -3 -8 -0.07 2.39 -9 -3 8 1.71 1.91 -9 3 8 4.29 1.29 9 3 -8 2.86 1.91 -7 -3 8 2.49 2.04 7 -3 -8 -0.01 2.23 -7 -3 8 4.52 1.27 -7 3 8 1.50 3.21 7 3 -8 4.83 1.87 -5 -3 8 6.11 2.97 -5 -3 8 0.05 1.11 -5 -3 8 1.44 0.70 5 -3 -8 0.15 1.35 -5 3 8 0.98 0.52 -5 3 8 3.55 2.70 5 3 -8 0.21 1.32 3 -3 -8 1.66 0.76 -3 -3 8 3.43 1.91 -3 -3 8 2.06 0.77 3 -3 -8 -0.05 1.25 3 3 -8 0.10 1.18 -3 3 8 0.91 0.46 1 -3 -8 4.69 1.06 1 3 -8 0.76 1.49 -1 3 8 2.85 1.88 1 -3 8 8.33 1.62 -1 -3 -8 4.91 0.90 3 -3 8 22.52 2.56 -5 -3 -8 3.53 1.61 5 -3 8 7.14 1.70 5 3 8 4.76 1.61 -5 3 -8 7.18 1.95 -7 -3 -8 0.06 0.86 -7 -3 -8 2.46 2.05 7 3 8 1.80 1.42 -7 3 -8 1.49 1.15 9 3 8 5.10 2.05 -9 3 -8 5.39 1.86 11 3 8 3.77 2.49 16 -4 -8 0.17 1.54 14 -4 -8 -0.16 1.31 12 -4 -8 -0.14 0.99 10 4 -8 1.58 1.68 8 -4 -8 -0.03 0.43 -8 -4 8 6.12 3.16 8 4 -8 0.37 1.31 -8 4 8 -1.71 2.80 -6 -4 8 6.30 1.18 -6 4 8 8.85 4.79 6 4 -8 8.89 2.56 4 4 -8 7.74 2.01 -4 4 8 9.19 4.10 2 -4 -8 13.57 1.30 2 4 -8 19.62 3.07 0 -4 -8 0.02 1.41 0 4 -8 1.41 1.93 -6 4 -8 4.83 1.74 -8 -4 -8 0.03 1.16 -16 0 9 3.40 1.82 -14 0 9 5.45 1.74 -12 0 9 0.49 1.10 -12 0 9 2.13 2.79 -10 0 9 -0.25 1.68 10 0 -9 1.55 1.59 10 0 -9 0.03 0.71 8 0 -9 2.17 1.54 -8 0 9 1.13 0.72 -8 0 9 -0.05 0.76 6 0 -9 2.34 1.28 -6 0 9 -0.10 0.84 6 0 -9 -0.07 1.00 -6 0 9 1.61 0.77 -4 0 9 -0.06 0.78 -4 0 9 0.43 0.58 -4 0 9 2.15 1.88 4 0 -9 -0.01 0.25 4 0 -9 -0.06 0.67 4 0 -9 0.76 1.13 2 0 -9 1.45 1.13 2 0 -9 -0.07 0.66 -2 0 9 3.23 2.08 -2 0 9 -0.05 0.64 2 0 -9 0.02 0.29 -2 0 9 0.58 0.53 0 0 -9 0.97 1.29 0 0 9 0.31 1.87 2 0 9 1.63 1.76 -2 0 -9 4.65 1.68 2 0 9 2.58 1.05 4 0 9 0.62 0.86 4 0 9 0.10 0.51 6 0 9 1.24 1.17 8 0 9 2.55 1.64 -10 0 -9 -0.36 1.00 10 0 9 1.07 1.38 10 0 9 0.00 0.71 -17 1 9 14.45 3.55 -15 -1 9 12.74 2.57 -13 1 9 11.61 2.16 -11 -1 9 -0.08 0.91 -11 -1 9 0.23 1.03 -11 1 9 0.46 1.02 -11 1 9 1.76 2.34 9 -1 -9 2.48 1.49 -9 1 9 2.54 2.71 9 1 -9 2.81 1.68 7 -1 -9 -0.04 0.92 7 -1 -9 2.52 1.35 -7 -1 9 2.72 2.00 -7 -1 9 0.19 0.96 -7 1 9 1.49 0.67 7 1 -9 2.23 1.58 -7 1 9 1.06 2.27 -5 -1 9 2.92 2.26 -5 1 9 3.82 1.80 -1 1 9 19.65 3.00 -1 1 9 15.16 1.90 1 1 -9 15.54 2.87 -1 -1 -9 20.92 2.56 1 -1 9 20.47 2.27 1 1 9 14.92 2.10 3 -1 9 0.11 0.82 3 -1 9 1.35 0.90 -3 -1 -9 -0.03 0.82 -3 1 -9 1.96 1.28 3 1 9 4.19 1.37 5 -1 9 1.93 1.13 5 1 9 1.36 1.10 7 -1 9 1.80 1.08 7 1 9 0.59 1.24 -9 -1 -9 8.34 2.17 9 1 9 12.09 2.70 -9 1 -9 14.68 2.18 -14 2 9 4.59 1.68 -12 -2 9 8.95 1.97 10 -2 -9 0.00 1.63 -10 -2 9 1.13 1.76 -10 2 9 5.38 3.52 10 2 -9 2.98 1.84 -8 -2 9 0.02 1.06 -8 -2 9 3.24 2.05 8 -2 -9 -0.02 1.63 -8 -2 9 2.11 0.92 -8 2 9 1.89 2.14 8 2 -9 0.66 1.42 -6 -2 9 8.59 1.51 6 -2 -9 10.94 1.87 -6 -2 9 6.14 2.45 -6 2 9 12.59 3.34 -6 2 9 10.35 1.30 6 2 -9 11.61 2.57 4 -2 -9 6.19 1.53 -4 -2 9 4.08 0.97 4 2 -9 4.58 1.53 -4 2 9 6.36 1.00 -2 -2 9 4.72 2.56 -2 -2 9 1.95 0.77 2 -2 -9 -0.04 0.81 -2 -2 9 -0.08 0.92 -2 2 9 1.22 0.58 -2 2 9 2.14 1.69 0 -2 9 4.52 1.43 -2 -2 -9 17.90 1.92 2 -2 9 22.18 2.50 2 2 9 15.59 2.13 -4 -2 -9 5.17 1.28 4 -2 9 6.42 1.68 -4 2 -9 4.37 1.65 -6 -2 -9 1.71 1.07 -6 -2 -9 0.02 0.70 6 2 9 0.80 1.11 -8 -2 -9 8.06 2.22 -8 2 -9 6.92 1.82 8 2 9 8.56 2.38 13 3 -9 4.74 2.36 11 3 -9 1.81 1.75 9 3 -9 3.76 1.93 -7 -3 9 10.23 3.72 7 3 -9 4.38 2.09 -7 3 9 5.85 3.53 5 3 -9 12.27 2.49 -5 3 9 19.42 4.01 -3 -3 9 5.76 2.30 -1 3 -9 10.70 3.12 -3 3 -9 9.76 2.83 -5 3 -9 6.54 2.14 -7 3 -9 4.49 1.68 10 -4 -9 -0.05 0.53 8 -4 -9 0.12 0.50 6 4 -9 3.03 1.52 4 4 -9 4.86 1.76 2 4 -9 7.15 2.50 0 4 -9 0.87 1.94 -2 -4 -9 0.05 0.43 -4 -4 -9 0.13 0.58 -12 0 10 10.50 2.20 12 0 -10 7.26 2.24 10 0 -10 3.47 1.78 -8 0 10 3.39 1.04 -6 0 10 15.25 1.82 4 0 -10 7.49 1.69 -4 0 10 7.24 1.24 -2 0 10 41.45 3.64 0 0 10 16.97 2.11 0 0 -10 19.87 3.04 2 0 10 3.44 1.16 -4 0 -10 3.73 1.32 4 0 10 5.09 1.54 -11 -1 10 6.84 1.77 -11 1 10 4.95 1.60 11 1 -10 7.93 2.62 -9 -1 10 5.49 1.41 9 -1 -10 6.08 1.86 -9 1 10 4.13 1.22 -7 -1 10 -0.10 1.06 -7 -1 10 1.44 0.78 7 1 -10 1.59 1.34 -7 1 10 1.47 0.72 5 -1 -10 1.91 1.19 -5 -1 10 0.00 1.01 -5 -1 10 0.99 0.70 5 1 -10 2.90 1.48 -5 1 10 1.62 0.61 -3 -1 10 5.38 1.13 3 -1 -10 5.62 1.43 3 1 -10 3.02 1.43 1 -1 -10 0.91 1.28 -1 -1 10 5.13 1.30 -1 1 10 2.79 0.98 1 1 -10 3.26 1.75 1 -1 10 3.40 1.10 1 1 10 2.61 1.02 -1 1 -10 5.92 2.03 3 -1 10 0.23 0.92 3 -1 10 1.06 0.86 -3 -1 -10 1.70 0.87 -3 1 -10 2.33 1.35 3 1 10 2.58 1.11 10 2 -10 10.48 2.90 8 2 -10 2.92 1.59 6 2 -10 2.99 1.65 2 2 -10 7.14 2.18 0 -2 -10 0.06 0.39 0 2 -10 0.90 1.64 -2 -2 -10 -0.03 0.46 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 71791 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn01 0.020(3) 0.024(2) 0.0205(18) -0.0013(16) -0.0040(16) 0.0029(16) O1 0.031(5) 0.025(4) 0.031(4) -0.002(3) -0.003(3) -0.001(3) O2 0.024(5) 0.028(4) 0.034(4) -0.001(3) -0.017(3) -0.005(3) O3 0.039(6) 0.023(4) 0.036(5) 0.004(4) -0.007(4) -0.007(4) C1 0.013(6) 0.016(4) 0.052(6) -0.007(4) -0.012(5) -0.003(3) C2 0.022(5) 0.017(4) 0.027(5) -0.001(3) -0.005(4) 0.000(3) C3 0.019(6) 0.015(4) 0.043(6) -0.002(4) -0.015(4) 0.003(3) C4 0.016(5) 0.024(4) 0.024(4) -0.005(3) -0.004(3) -0.005(3) loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn01 Mn Uani 0.25000 0.25000 0.00000 1.000 0.0223(13) d SP . . O1 O Uani 0.1828(6) 0.3410(13) 0.2018(12) 1.000 0.030(3) d U . . O2 O Uani 0.1704(5) 0.6681(13) 0.2678(12) 1.000 0.031(3) d U . . O3 O Uani 0.1944(6) -0.0452(14) -0.0170(13) 1.000 0.034(3) d . . . C1 C Uani 0.0336(6) 0.6837(14) 0.0578(16) 1.000 0.029(3) d U . . C2 C Uani 0.0683(6) 0.5010(13) 0.0935(13) 1.000 0.023(3) d U . . C3 C Uani 0.0377(6) 0.3197(14) 0.0360(15) 1.000 0.028(3) d U . . C4 C Uani 0.1457(6) 0.5034(14) 0.1964(13) 1.000 0.022(3) d U . . H1 H Uiso 0.192(4) -0.134(11) -0.115(9) 1.000 0.0510 d U . . H1A H Uiso 0.182(4) -0.120(10) 0.086(9) 1.000 0.0510 d U . . H1B H Uiso 0.05659 0.80585 0.09469 1.000 0.0350 c RU . . H3 H Uiso 0.06376 0.19936 0.05871 1.000 0.0340 c RU . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn01 O3 87.8(4) . . . yes O1 Mn01 O2 94.2(5) . . 4_564 yes O1 Mn01 O2 85.8(5) . . 6_545 yes O1 Mn01 O1 180.00 . . 7_555 yes O1 Mn01 O3 92.2(4) . . 7_555 yes O2 Mn01 O3 85.1(4) 4_564 . . yes O2 Mn01 O3 94.9(4) 6_545 . . yes O1 Mn01 O3 92.2(4) 7_555 . . yes O3 Mn01 O3 180.00 . . 7_555 yes O2 Mn01 O2 180.00 4_564 . 6_545 yes O1 Mn01 O2 85.8(5) 7_555 . 4_564 yes O2 Mn01 O3 94.9(4) 4_564 . 7_555 yes O1 Mn01 O2 94.2(5) 7_555 . 6_545 yes O2 Mn01 O3 85.1(4) 6_545 . 7_555 yes O1 Mn01 O3 87.8(4) 7_555 . 7_555 yes Mn01 O1 C4 125.6(7) . . . yes Mn01 O2 C4 135.2(7) 4_565 . . yes H1 O3 H1A 108(6) . . . no Mn01 O3 H1 124(5) . . . no Mn01 O3 H1A 125(4) . . . no C2 C1 C3 117.7(9) . . 3_565 no C3 C2 C4 118.9(9) . . . no C1 C2 C3 123.0(11) . . . no C1 C2 C4 118.0(9) . . . no C1 C3 C2 119.2(9) 3_565 . . no O1 C4 O2 123.2(11) . . . yes O1 C4 C2 118.6(9) . . . yes O2 C4 C2 118.2(9) . . . yes C2 C1 H1B 121.00 . . . no C3 C1 H1B 121.00 3_565 . . no C2 C3 H3 120.00 . . . no C1 C3 H3 120.00 3_565 . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn01 O1 2.180(14) . . yes Mn01 O3 2.195(14) . . yes Mn01 O2 2.148(13) . 4_564 yes Mn01 O2 2.148(13) . 6_545 yes Mn01 O1 2.180(14) . 7_555 yes Mn01 O3 2.195(14) . 7_555 yes O1 C4 1.270(15) . . yes O2 C4 1.258(14) . . yes O3 H1 0.92(7) . . no O3 H1A 0.96(7) . . no C1 C2 1.370(15) . . no C1 C3 1.400(17) . 3_565 no C2 C4 1.523(17) . . no C2 C3 1.359(15) . . no C1 H1B 0.9300 . . no C3 H3 0.9300 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O3 H1 O1 0.92(7) 1.91(7) 2.824(18) 173(8) 4_554 yes O3 H1A O2 0.96(7) 1.97(7) 2.908(19) 165(6) 1_545 yes C3 H3 O1 0.9300 2.4900 2.80(2) 100.00 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn01 O1 C4 -129.0(10) . . . . no O2 Mn01 O1 C4 -44.1(10) 4_564 . . . no O2 Mn01 O1 C4 135.9(10) 6_545 . . . no O3 Mn01 O1 C4 51.0(10) 7_555 . . . no Mn01 O1 C4 O2 -89.1(12) . . . . no Mn01 O1 C4 C2 88.9(12) . . . . no Mn01 O2 C4 O1 -30.5(17) 4_565 . . . no Mn01 O2 C4 C2 151.4(8) 4_565 . . . no C3 C1 C2 C3 2.6(17) 3_565 . . . no C3 C1 C2 C4 -179.7(10) 3_565 . . . no C2 C1 C3 C2 -2.5(16) . . 3_565 3_565 no C1 C2 C3 C1 -2.7(17) . . . 3_565 no C4 C2 C3 C1 179.6(10) . . . 3_565 no C1 C2 C4 O1 -167.6(10) . . . . no C1 C2 C4 O2 10.5(14) . . . . no C3 C2 C4 O1 10.2(15) . . . . no C3 C2 C4 O2 -171.7(10) . . . . no