#------------------------------------------------------------------------------ #$Date: 2021-07-09 11:17:25 +0300 (Fri, 09 Jul 2021) $ #$Revision: 267421 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/40/1564076.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1564076 loop_ _publ_author_name '\'Swiderski, Grzegorz' '\/Lyszczek, Renata' 'Wojtulewski, S\/lawomir' 'Kalinowska, Monika' '\'Swis\/locka, Renata' 'Lewandowski, W\/lodzimierz' _publ_section_title ; Comparison of structural, spectroscopic, theoretical and thermal properties of metal complexes (Zn(II), Mn(II), Cu(II), Ni(II) and Co(II)) of pyridazine-3-carboxylic acid and pyridazine-4-carboxylic acids ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119865 _journal_paper_doi 10.1016/j.ica.2020.119865 _journal_volume 512 _journal_year 2020 _chemical_formula_moiety '0.5(C10 H14 Mn N4 O8), H2 O' _chemical_formula_sum 'C5 H9 Mn0.5 N2 O5' _chemical_formula_weight 204.61 _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 97.344(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.1170(10) _cell_length_b 6.7745(3) _cell_length_c 6.2323(4) _cell_measurement_reflns_used 4033 _cell_measurement_temperature 100 _cell_measurement_theta_max 77.1890 _cell_measurement_theta_min 4.6720 _cell_volume 800.51(8) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4052 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -11.00 38.00 1.00 1.00 -- 43.67 77.00 -90.00 49 2 \w 49.00 107.00 1.00 1.00 -- 43.67 77.00 -90.00 58 3 \w 112.00 150.00 1.00 1.00 -- 43.67 77.00 -90.00 38 4 \w 135.00 176.00 1.00 1.00 -- 87.33 104.00 -90.00 41 5 \w 140.00 166.00 1.00 1.00 -- 87.33 155.00 -43.00 26 6 \w 134.00 168.00 1.00 1.00 -- 87.33 104.00-150.00 34 7 \w 141.00 174.00 1.00 1.00 -- 131.00 77.00 -90.00 33 8 \w 148.00 174.00 1.00 1.00 -- 131.00 77.00-180.00 26 9 \w 120.00 146.00 1.00 1.00 -- 131.00 99.00-180.00 26 10 \w 106.00 161.00 1.00 1.00 -- 131.00 77.00-150.00 55 11 \w 102.00 177.00 1.00 1.00 -- 87.33 104.00 -30.00 75 12 \w 140.00 175.00 1.00 1.00 -- 131.00 43.00 60.00 35 13 \w 152.00 177.00 1.00 1.00 -- 131.00 77.00 30.00 25 14 \w 138.00 164.00 1.00 1.00 -- 98.00 51.00 90.23 26 15 \w 139.00 165.00 1.00 1.00 -- 131.00 65.00 150.00 26 16 \w 113.00 138.00 1.00 1.00 -- 131.00 120.00 158.00 25 17 \w 111.00 149.00 1.00 1.00 -- 131.00 99.00 150.00 38 18 \w 127.00 165.00 1.00 1.00 -- 87.33 138.00 60.00 38 19 \w 125.00 177.00 1.00 1.00 -- 131.00 77.00 -30.00 52 20 \w 115.00 167.00 1.00 1.00 -- 131.00 125.00 60.00 52 21 \w 107.00 162.00 1.00 1.00 -- 131.00 77.00 120.00 55 22 \w 93.00 123.00 1.00 1.00 -- 87.33 138.00 60.00 30 23 \w 94.00 149.00 1.00 1.00 -- 43.67 125.00 60.00 55 24 \w 88.00 113.00 1.00 1.00 -- 43.67 155.00 -43.00 25 25 \w 74.00 173.00 1.00 1.00 -- 87.33 77.00 30.00 99 26 \w 112.00 138.00 1.00 1.00 -- 131.00 178.00-120.00 26 27 \w 87.00 138.00 1.00 1.00 -- 131.00 178.00 -90.00 51 28 \w 78.00 128.00 1.00 1.00 -- 131.00 155.00 -43.00 50 29 \w 78.00 104.00 1.00 1.00 -- 131.00 77.00 -30.00 26 30 \w 78.00 121.00 1.00 1.00 -- 131.00 65.00 -60.00 43 31 \w 81.00 178.00 1.00 1.00 -- 131.00 65.00 0.00 97 32 \w 81.00 123.00 1.00 1.00 -- 131.00 65.00 60.00 42 33 \w 76.00 140.00 1.00 1.00 -- 131.00 77.00 60.00 64 34 \w 76.00 127.00 1.00 1.00 -- 131.00 65.00 -30.00 51 35 \w 78.00 139.00 1.00 1.00 -- 131.00 65.00-120.00 61 36 \w 81.00 121.00 1.00 1.00 -- 131.00 77.00-180.00 40 37 \w 77.00 127.00 1.00 1.00 -- 131.00 65.00-180.00 50 38 \w 78.00 139.00 1.00 1.00 -- 131.00 77.00 -90.00 61 39 \w 77.00 115.00 1.00 1.00 -- 131.00 65.00-150.00 38 40 \w 77.00 102.00 1.00 1.00 -- 131.00 77.00-150.00 25 41 \w 78.00 147.00 1.00 1.00 -- 131.00 77.00-120.00 69 42 \w 76.00 119.00 1.00 1.00 -- 131.00 65.00 -90.00 43 43 \w 77.00 132.00 1.00 1.00 -- 131.00 77.00 -60.00 55 44 \w 76.00 146.00 1.00 1.00 -- 131.00 77.00 30.00 70 45 \w 77.00 118.00 1.00 1.00 -- 131.00 65.00 90.00 41 46 \w 78.00 132.00 1.00 1.00 -- 131.00 65.00 120.00 54 47 \w 76.00 178.00 1.00 1.00 -- 131.00 77.00 90.00 102 48 \w 76.00 132.00 1.00 1.00 -- 131.00 77.00 150.00 56 49 \w 76.00 102.00 1.00 1.00 -- 131.00 77.00 120.00 26 50 \w 76.00 115.00 1.00 1.00 -- 131.00 65.00 150.00 39 51 \w 69.00 97.00 1.00 1.00 -- 131.00 43.00 60.00 28 52 \w 43.00 71.00 1.00 1.00 -- 98.00 77.00 -23.02 28 53 \w 32.00 58.00 1.00 1.00 -- 87.33 77.00 60.00 26 54 \w 40.00 123.00 1.00 1.00 -- 98.00 51.00 90.23 83 55 \w 38.00 79.00 1.00 1.00 -- 98.00 49.00 138.44 41 56 \w 33.00 69.00 1.00 1.00 -- 87.33 77.00 30.00 36 57 \w 15.00 43.00 1.00 1.00 -- 70.00 82.00 96.58 28 58 \w 5.00 32.00 1.00 1.00 -- 62.00 90.00 166.81 27 59 \w -2.00 23.00 1.00 1.00 -- 58.00 96.00 52.92 25 60 \w 5.00 30.00 1.00 1.00 -- 62.00 90.00 9.79 25 61 \w 6.00 32.00 1.00 1.00 -- 62.00 89.00 -10.66 26 62 \w -1.00 26.00 1.00 1.00 -- 58.00 93.00 -50.81 27 63 \w -9.00 16.00 1.00 1.00 -- 54.00 104.00-111.96 25 64 \w 34.00 61.00 1.00 1.00 -- 87.33 77.00-150.00 27 65 \w 35.00 77.00 1.00 1.00 -- 94.00 50.00 -66.71 42 66 \w 23.00 178.00 1.00 1.00 -- 131.00 -32.00 0.00 155 67 \w 107.00 173.00 1.00 1.00 -- 131.00 -89.00-120.00 66 68 \w 122.00 169.00 1.00 1.00 -- 131.00 -77.00-150.00 47 69 \w 88.00 133.00 1.00 1.00 -- 131.00-155.00 -82.00 45 70 \w 77.00 102.00 1.00 1.00 -- 131.00 -99.00 0.00 25 71 \w 58.00 119.00 1.00 1.00 -- 131.00-120.00 75.00 61 72 \w 144.00 178.00 1.00 1.00 -- 131.00 -89.00 150.00 34 73 \w 55.00 104.00 1.00 1.00 -- 131.00 -99.00 90.00 49 74 \w 55.00 156.00 1.00 1.00 -- 131.00 -65.00 30.00 101 75 \w 72.00 97.00 1.00 1.00 -- 131.00 -77.00-150.00 25 76 \w 51.00 88.00 1.00 1.00 -- 131.00 -89.00-120.00 37 77 \w 54.00 96.00 1.00 1.00 -- 131.00 -99.00-150.00 42 78 \w 25.00 107.00 1.00 1.00 -- 131.00 -99.00 -90.00 82 79 \w 34.00 60.00 1.00 1.00 -- 131.00 -99.00 0.00 26 80 \w 28.00 54.00 1.00 1.00 -- 131.00-120.00 75.00 26 81 \w 52.00 78.00 1.00 1.00 -- 131.00 -89.00 150.00 26 82 \w 50.00 83.00 1.00 1.00 -- 43.67-120.00 75.00 33 83 \w 21.00 46.00 1.00 1.00 -- 0.00-120.00 75.00 25 84 \w 7.00 51.00 1.00 1.00 -- 0.00 -99.00 0.00 44 85 \w 2.00 48.00 1.00 1.00 -- 0.00 -99.00 -30.00 46 86 \w 10.00 60.00 1.00 1.00 -- 0.00 -99.00-120.00 50 87 \w -56.00 -31.00 1.00 1.00 -- -86.50 -77.00 30.00 25 88 \w -62.00 -33.00 1.00 1.00 -- -86.50 -77.00 -30.00 29 89 \w -61.00 -35.00 1.00 1.00 -- -86.50 -72.00 3.00 26 90 \w -59.00 -33.00 1.00 1.00 -- -86.50 -77.00 -60.00 26 91 \w -66.00 -33.00 1.00 1.00 -- -86.50 -75.00 -82.75 33 92 \w -58.00 -33.00 1.00 1.00 -- -86.50 -77.00-120.00 25 93 \w -61.00 -31.00 1.00 1.00 -- -86.50 -77.00-168.90 30 94 \w -61.00 -31.00 1.00 1.00 -- -86.50 -77.00-150.00 30 95 \w -86.00 -60.00 1.00 1.00 -- -43.67-155.00 -82.00 26 96 \w -106.00 -81.00 1.00 1.00 -- 0.00-155.00 -82.00 25 97 \w -134.00 -80.00 1.00 1.00 -- -43.67 -99.00-150.00 54 98 \w -117.00 -75.00 1.00 1.00 -- -86.50 -77.00-150.00 42 99 \w -92.00 -67.00 1.00 1.00 -- -86.50 -77.00-168.90 25 100 \w -129.00 -81.00 1.00 1.00 -- -86.50-104.00-150.00 48 101 \w -145.00-110.00 1.00 1.00 -- -86.50-155.00 -82.00 35 102 \w -152.00-102.00 1.00 1.00 -- -43.67 -99.00 -60.00 50 103 \w -109.00 0.00 1.00 1.00 -- -43.67 -57.00 0.00 109 104 \w -63.00 -21.00 1.00 1.00 -- -43.67 -57.00 90.00 42 105 \w -65.00 -35.00 1.00 1.00 -- -86.50 -77.00 73.63 30 106 \w -64.00 -31.00 1.00 1.00 -- -86.50 -77.00 98.92 33 107 \w -79.00 50.00 1.00 1.00 -- -43.67 -19.00 120.00 129 108 \w -53.00 -28.00 1.00 1.00 -- -86.50 120.00 158.00 25 109 \w -48.00 -18.00 1.00 1.00 -- 0.00 120.00 158.00 30 110 \w -30.00 -5.00 1.00 1.00 -- 43.67 123.00-174.66 25 111 \w -89.00 -64.00 1.00 1.00 -- -86.50 155.00 -43.00 25 112 \w -142.00 -83.00 1.00 1.00 -- -43.67 -19.00 120.00 59 113 \w -125.00 -88.00 1.00 1.00 -- -43.67 -57.00 90.00 37 114 \w -134.00 -87.00 1.00 1.00 -- -43.67 -99.00 90.00 47 115 \w -99.00 -33.00 1.00 1.00 -- -86.50 -73.00 123.91 66 116 \w -142.00-106.00 1.00 1.00 -- -86.50 -77.00 73.63 36 117 \w -149.00 -82.00 1.00 1.00 -- -43.67-120.00 75.00 67 118 \w -146.00 -73.00 1.00 1.00 -- -86.50 -77.00 -30.00 73 119 \w -151.00-126.00 1.00 1.00 -- -86.50-120.00 75.00 25 120 \w -154.00 -76.00 1.00 1.00 -- -86.50 -77.00 30.00 78 121 \w -146.00 -97.00 1.00 1.00 -- -86.50 -75.00 -82.75 49 122 \w -160.00-135.00 1.00 1.00 -- -86.50-104.00-150.00 25 123 \w -167.00-141.00 1.00 1.00 -- -86.50 -77.00-150.00 26 124 \w -177.00 -74.00 1.00 1.00 -- -86.50 -77.00-120.00 103 125 \w -177.00 -77.00 1.00 1.00 -- -86.50 -77.00 -60.00 100 126 \w -176.00-122.00 1.00 1.00 -- -86.50 -73.00 123.91 54 127 \w -140.00 -41.00 1.00 1.00 -- -86.50 -64.00 150.00 99 128 \w -176.00 -75.00 1.00 1.00 -- -86.50 -72.00 3.00 101 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0360690000 _diffrn_orient_matrix_UB_12 0.1929783000 _diffrn_orient_matrix_UB_13 -0.0569584000 _diffrn_orient_matrix_UB_21 -0.0721911000 _diffrn_orient_matrix_UB_22 0.1041303000 _diffrn_orient_matrix_UB_23 -0.0337180000 _diffrn_orient_matrix_UB_31 0.0091810000 _diffrn_orient_matrix_UB_32 0.0603530000 _diffrn_orient_matrix_UB_33 0.2402638000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1652 _diffrn_reflns_av_unetI/netI 0.0966 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 5708 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.450 _diffrn_reflns_theta_min 4.664 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.306 _exptl_absorpt_correction_T_max 0.557 _exptl_absorpt_correction_T_min 0.151 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.698 _exptl_crystal_description block _exptl_crystal_F_000 422 _exptl_crystal_size_max 0.335 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.089 _refine_diff_density_max 0.791 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.313 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 78 _refine_ls_number_reflns 891 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.119 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0866 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1669P)^2^+3.1476P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2056 _refine_ls_wR_factor_ref 0.2428 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 860 _reflns_number_total 891 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_3224_twin1_hklf4_a.res in C2/m exp_3224_twin1_hklf4.res created by SHELXL-2018/3 at 14:15:37 on 02-Apr-2020 REM Old TITL exp_3224_twin1_hklf4 in C2/m REM SHELXT solution in C2/m: R1 0.201, Rweak 0.070, Alpha 0.072 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C16 N6 O2 Mn CELL 1.54184 19.117 6.7745 6.2323 90 97.344 90 ZERR 4 0.001 0.0003 0.0004 0 0.005 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Mn N O UNIT 20 36 2 8 20 EQIV $1 0.5+X,0.5+Y,+Z EQIV $2 +X,+Y,1+Z FLAT C5 C4 C7 O2 H2Wa O2W H2Wb L.S. 10 PLAN 1 SIZE 0.089 0.26 0.335 TEMP -173.15 HTAB O1W O1_$1 HTAB O2W O1_$2 HTAB O2W O2 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.166900 3.147600 FVAR 0.20216 MN1 3 0.500000 0.500000 0.000000 10.25000 0.01653 0.02984 = 0.02425 0.00000 0.00745 0.00000 O1W 5 0.531362 0.728635 0.243729 11.00000 0.02657 0.03699 = 0.03527 -0.00657 0.00662 -0.00401 AFIX 7 H1WA 2 0.499591 0.823282 0.237484 11.00000 -1.50000 H1WB 2 0.569501 0.791809 0.215986 11.00000 -1.50000 AFIX 6 O2W 5 0.074309 0.500000 0.733535 10.50000 0.02399 0.05218 = 0.03364 0.00000 0.01110 0.00000 H2WA 2 0.104210 0.500000 0.643617 10.50000 -1.50000 H2WB 2 0.097478 0.500000 0.858496 10.50000 -1.50000 AFIX 0 O1 5 0.135222 0.500000 0.158870 10.50000 0.01898 0.06200 = 0.04205 0.00000 0.00735 0.00000 O2 5 0.182765 0.500000 0.502138 10.50000 0.03064 0.11152 = 0.03568 0.00000 0.01695 0.00000 N1 4 0.392644 0.500000 0.112575 10.50000 0.01542 0.04146 = 0.02453 0.00000 0.00713 0.00000 N2 4 0.335256 0.500000 -0.040783 10.50000 0.01974 0.05352 = 0.02360 0.00000 0.00470 0.00000 C4 1 0.260061 0.500000 0.239762 10.50000 0.01726 0.03067 = 0.02567 0.00000 0.00772 0.00000 C3 1 0.271959 0.500000 0.022401 10.50000 0.01998 0.04633 = 0.02289 0.00000 0.00279 0.00000 AFIX 43 H3 2 0.232128 0.500000 -0.085693 10.50000 -1.20000 AFIX 0 C5 1 0.318443 0.500000 0.392013 10.50000 0.02190 0.04656 = 0.02321 0.00000 0.00593 0.00000 AFIX 43 H5 2 0.314100 0.500000 0.542168 10.50000 -1.20000 AFIX 0 C7 1 0.187289 0.500000 0.306409 10.50000 0.02107 0.03842 = 0.03807 0.00000 0.01425 0.00000 C6 1 0.384408 0.500000 0.319472 10.50000 0.01994 0.05391 = 0.02562 0.00000 0.00594 0.00000 AFIX 43 H6 2 0.425280 0.500000 0.423667 10.50000 -1.20000 AFIX 0 HKLF 4 REM exp_3224_twin1_hklf4_a.res in C2/m REM wR2 = 0.2428, GooF = S = 1.122, Restrained GooF = 1.119 for all data REM R1 = 0.0866 for 860 Fo > 4sig(Fo) and 0.1073 for all 891 data REM 78 parameters refined using 4 restraints END WGHT 0.1669 3.1477 REM Highest difference peak 0.791, deepest hole -1.229, 1-sigma level 0.313 Q1 1 0.4996 0.5000 0.2057 10.50000 0.05 0.79 REM The information below was added by Olex2. REM REM R1 = 0.0866 for 860 Fo > 4sig(Fo) and 0.1073 for all 5708 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.79, deepest hole -1.23 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1073 REM R1_gt = 0.0866 REM wR_ref = 0.2428 REM GOOF = 1.122 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 5708 REM Reflections_gt = 860 REM Parameters = n/a REM Hole = -1.23 REM Peak = 0.79 REM Flack = n/a ; _cod_data_source_file ICA-2020-512-119865.cif _cod_data_source_block exp_3224_twin1_hklf4 _cod_original_formula_sum 'C5 H9 Mn0.50 N2 O5' _cod_database_code 1564076 _chemical_oxdiff_formula 'C20 H36 Mn2 N8 O20 ' _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_max 0.562 _shelx_estimated_absorpt_t_min 0.193 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Restrained planarity C5, C4, C7, O2, H2WA, O2W, H2WB with sigma of 0.1 3.a Free rotating group: O2W(H2WA,H2WB) 3.b Rotating group: O1W(H1WA,H1WB) 3.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C6(H6) ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.500000 0.500000 0.000000 0.0231(5) Uani 1 4 d S T P . . O1W O 0.53136(18) 0.7286(6) 0.2437(5) 0.0327(9) Uani 1 1 d . . . . . H1WA H 0.499591 0.823282 0.237484 0.049 Uiso 1 1 d GR . . . . H1WB H 0.569501 0.791809 0.215986 0.049 Uiso 1 1 d GR . . . . O2W O 0.0743(3) 0.500000 0.7335(9) 0.0360(12) Uani 1 2 d S T P . . H2WA H 0.104210 0.500000 0.643617 0.054 Uiso 1 2 d GS T P . . H2WB H 0.097478 0.500000 0.858496 0.054 Uiso 1 2 d GS T P . . O1 O 0.1352(3) 0.500000 0.1589(10) 0.0407(14) Uani 1 2 d S T P . . O2 O 0.1828(3) 0.500000 0.5021(10) 0.058(2) Uani 1 2 d S T P . . N1 N 0.3926(3) 0.500000 0.1126(9) 0.0267(12) Uani 1 2 d S T P . . N2 N 0.3353(3) 0.500000 -0.0408(9) 0.0321(14) Uani 1 2 d S T P . . C4 C 0.2601(3) 0.500000 0.2398(10) 0.0241(13) Uani 1 2 d S T P . . C3 C 0.2720(4) 0.500000 0.0224(11) 0.0297(15) Uani 1 2 d S T P . . H3 H 0.232128 0.500000 -0.085693 0.036 Uiso 1 2 calc RS T P . . C5 C 0.3184(4) 0.500000 0.3920(11) 0.0303(15) Uani 1 2 d S T P . . H5 H 0.314100 0.500000 0.542168 0.036 Uiso 1 2 calc RS T P . . C7 C 0.1873(4) 0.500000 0.3064(12) 0.0316(15) Uani 1 2 d S T P . . C6 C 0.3844(4) 0.500000 0.3195(11) 0.0329(16) Uani 1 2 d S T P . . H6 H 0.425280 0.500000 0.423667 0.039 Uiso 1 2 calc RS T P . . 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 Mn1 0.0165(8) 0.0298(8) 0.0243(8) 0.000 0.0074(5) 0.000 O1W 0.0266(17) 0.037(2) 0.0353(18) -0.0066(14) 0.0066(13) -0.0040(14) O2W 0.024(2) 0.052(3) 0.034(3) 0.000 0.011(2) 0.000 O1 0.019(2) 0.062(4) 0.042(3) 0.000 0.007(2) 0.000 O2 0.031(3) 0.112(6) 0.036(3) 0.000 0.017(2) 0.000 N1 0.015(3) 0.041(3) 0.025(3) 0.000 0.007(2) 0.000 N2 0.020(3) 0.054(4) 0.024(3) 0.000 0.005(2) 0.000 C4 0.017(3) 0.031(3) 0.026(3) 0.000 0.008(2) 0.000 C3 0.020(3) 0.046(4) 0.023(3) 0.000 0.003(2) 0.000 C5 0.022(3) 0.047(4) 0.023(3) 0.000 0.006(2) 0.000 C7 0.021(3) 0.038(4) 0.038(4) 0.000 0.014(3) 0.000 C6 0.020(3) 0.054(4) 0.026(3) 0.000 0.006(2) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 4 0 0.1507 -1 -1 4 0.1248 -2 -4 0 0.1507 12 0 0 0.0620 -12 0 0 0.0270 1 0 -4 0.1299 -1 0 4 0.1299 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_3 O1W Mn1 O1W 90.4(2) 5_665 6_565 O1W Mn1 O1W 89.6(2) 6_565 . O1W Mn1 O1W 180.0 5_665 . O1W Mn1 O1W 89.6(2) 5_665 2_655 O1W Mn1 O1W 180.00(13) 6_565 2_655 O1W Mn1 O1W 90.4(2) 2_655 . O1W Mn1 N1 92.08(14) . 5_665 O1W Mn1 N1 92.08(14) 6_565 5_665 O1W Mn1 N1 87.92(14) 5_665 5_665 O1W Mn1 N1 87.92(14) 6_565 . O1W Mn1 N1 87.92(14) 2_655 5_665 O1W Mn1 N1 87.92(14) . . O1W Mn1 N1 92.08(14) 5_665 . O1W Mn1 N1 92.08(14) 2_655 . N1 Mn1 N1 180.0 . 5_665 Mn1 O1W H1WA 110.9 . . Mn1 O1W H1WB 111.5 . . H1WA O1W H1WB 102.8 . . H2WA O2W H2WB 106.9 . . N2 N1 Mn1 117.8(4) . . C6 N1 Mn1 122.1(4) . . C6 N1 N2 120.1(5) . . C3 N2 N1 118.6(6) . . C3 C4 C7 122.5(6) . . C5 C4 C3 116.8(6) . . C5 C4 C7 120.7(6) . . N2 C3 C4 123.8(6) . . N2 C3 H3 118.1 . . C4 C3 H3 118.1 . . C4 C5 H5 121.1 . . C4 C5 C6 117.8(6) . . C6 C5 H5 121.1 . . O1 C7 C4 118.0(6) . . O2 C7 O1 124.8(7) . . O2 C7 C4 117.3(7) . . N1 C6 C5 122.9(6) . . N1 C6 H6 118.5 . . C5 C6 H6 118.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 O1W 2.198(3) 5_665 Mn1 O1W 2.198(3) . Mn1 O1W 2.198(3) 6_565 Mn1 O1W 2.198(3) 2_655 Mn1 N1 2.252(6) 5_665 Mn1 N1 2.252(6) . O1W H1WA 0.8806 . O1W H1WB 0.8814 . O2W H2WA 0.8501 . O2W H2WB 0.8453 . O1 C7 1.266(10) . O2 C7 1.234(9) . N1 N2 1.360(8) . N1 C6 1.319(8) . N2 C3 1.320(9) . C4 C3 1.402(9) . C4 C5 1.369(9) . C4 C7 1.502(9) . C3 H3 0.9500 . C5 H5 0.9500 . C5 C6 1.393(10) . C6 H6 0.9500 . 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 O1W H1WB O1 0.88 1.95 2.805(6) 162.7 3 yes O2W H2WA O2 0.85 1.84 2.673(8) 167.6 . yes O2W H2WB O1 0.85 1.92 2.756(8) 170.6 1_556 yes loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 3 1 -4 60.5 0.34 4 2 -4 9.05 0.17 2 0 -4 16.88 0.19 2 2 -4 9.55 0.16 1 1 -4 5.95 0.13 0 0 -4 141.29 0.52 0 2 -4 8.76 0.15 -1 1 -4 3.26 0.11 -2 0 -4 63.19 0.34 -2 2 -4 0.97 0.09 -3 1 -4 22.16 0.21 -4 0 -4 228.21 0.61 2 2 -3 49.88 0.56 1 -1 -3 94.39 0.63 0 0 -3 39.6 0.44 0 2 -1 81.07 0.42 0 2 -2 166.61 0.8 0 2 -3 51.77 0.56 -1 1 -2 134.71 0.69 -1 1 -1 613.96 1.08 -1 1 -3 95.79 0.72 -2 0 -3 39.37 0.45 -1 -1 -2 138.52 0.59 -2 0 -2 217.98 0.85 -2 2 -3 7.29 0.24 -2 2 -2 24.84 0.33 -3 1 -3 20.05 0.35 -3 1 -2 73.21 0.55 -2 2 -1 217.12 0.72 -4 0 -3 85.2 0.71 -4 2 -3 3.17 0.19 -3 3 -3 8.92 0.28 -3 1 -1 7.05 0.14 -5 1 -3 79.88 0.75 -4 2 -2 195.61 0.98 -4 0 -2 15.83 0.26 -3 -1 -2 73.59 0.48 -5 1 -2 34.47 0.42 -6 2 -3 1.62 0.18 -6 0 -3 82.6 0.77 -4 2 -1 332.58 1.06 -4 0 -1 63.99 0.41 -7 1 0 -15.38 0.86 -6 0 0 -96.17 1.3 -8 2 0 22.44 0.53 -9 1 0 51.04 1.42 -8 0 0 -2.49 0.57 -10 2 0 150.43 0.9 -11 1 0 13.47 0.33 -10 0 0 14.28 0.62 -5 -1 0 -47.21 0.94 -7 -1 0 -23.83 0.98 -12 2 0 184.1 1.01 -12 0 0 59.26 0.64 -13 1 0 31.29 0.49 -9 -1 0 -165.33 1.57 -11 -1 0 2.72 0.37 -13 -1 0 24.31 0.49 -6 0 -1 35.8 0.43 -8 0 -2 12.42 0.35 -7 1 -1 3.55 0.18 -9 1 -2 39.52 0.67 -7 -1 -2 8.67 0.28 -5 -1 -1 34.73 0.41 -8 2 -1 140.53 1.08 -10 2 -2 17.35 0.5 -8 0 -1 1.55 0.15 -9 1 -1 72.14 0.78 -10 0 -2 55.09 0.81 -11 1 -2 26.02 0.61 -9 -1 -2 33.49 0.57 -7 -1 -1 4.07 0.19 -10 2 -1 27.52 0.53 -10 0 -1 21.26 0.44 -11 1 -1 114.93 1.07 -9 -1 -1 85.91 0.8 -12 2 -1 35.01 0.63 -12 0 -1 2.55 0.23 -11 -1 -1 124.03 1.05 -13 -1 -1 21.23 0.48 -7 1 1 90.5 0.75 -9 1 1 2.38 0.17 -11 1 1 19.74 0.42 -8 0 1 1231.8 2.93 -10 0 1 66.49 0.73 -5 1 1 475.2 1.38 -6 0 1 108.78 0.74 -13 1 1 26.25 0.5 -12 0 1 58.03 0.73 -9 -1 1 1.75 0.19 -11 -1 1 22.04 0.48 -5 -1 1 476.25 1.38 -11 1 2 22.54 0.5 -10 -2 1 7.25 0.29 -13 1 2 174.98 1.34 -12 -2 1 2.96 0.24 -12 0 2 58.83 0.8 -9 1 2 1.39 0.16 -10 0 2 64.56 0.78 -8 -2 1 241.65 1.32 -8 0 2 66.44 0.71 -11 -1 2 19.64 0.5 -13 -1 2 186.58 1.5 -7 1 2 134.02 0.91 -9 -1 2 1.36 0.17 -6 -2 1 38.03 0.45 -6 0 2 123.75 0.82 -7 -1 2 129.72 0.96 -12 -2 2 1.35 0.23 -3 -1 1 34.22 0.29 -10 -2 2 8.21 0.34 -5 1 2 12.05 0.24 -11 1 3 2.44 0.24 -10 0 3 0.71 0.19 -8 -2 2 43.23 0.64 -9 1 3 58.19 0.77 -5 -1 2 11.96 0.26 -8 0 3 1.06 0.19 -4 0 2 1.35 0.1 -9 -1 3 59.48 0.84 -7 1 3 94.81 0.87 -6 -2 2 172.94 1.09 -10 -2 3 44.43 0.8 -7 -1 3 93.7 0.95 -6 0 3 3.41 0.2 -3 1 2 1.41 0.09 -8 -2 3 67.28 0.9 -5 1 3 42.1 0.52 -3 -1 2 1.31 0.09 -4 -2 2 108.28 0.76 -8 0 4 8.77 0.2 -8 -2 4 18.11 0.29 -7 -1 4 94.05 0.51 -9 1 4 72.09 0.44 -6 0 4 82.39 0.46 -6 -2 4 32.33 0.34 -7 1 4 92.45 0.48 -13 -1 5 10.72 0.52 -15 -1 5 19.34 0.54 -5 -1 4 29.49 0.3 -14 0 5 20.95 0.69 -11 -1 5 31.13 0.8 -12 0 5 55.36 1.08 -14 -2 5 23.33 0.63 -12 -2 5 39.85 0.82 -10 0 5 12.73 0.51 -9 -1 5 189.38 1.68 -10 -2 5 53.22 0.97 -5 1 4 31.49 0.29 -11 1 5 27.37 0.8 -8 0 5 131.78 1.41 -4 -2 4 11.38 0.21 -8 -2 5 89.65 1.17 -7 -1 5 26.32 0.66 -9 1 5 219.13 1.68 -6 0 5 49.52 0.85 -6 -2 5 15.47 0.54 -7 1 5 29.27 0.67 -5 -1 5 50.04 0.84 -2 -2 4 9.84 0.2 -11 -1 6 6.35 0.18 -4 0 5 77.55 0.98 -10 0 6 11.14 0.23 -5 1 5 48.41 0.82 -9 -1 6 14.37 0.25 -4 -2 5 10.09 0.44 -3 -1 5 104.67 1.13 -8 0 6 12.03 0.25 -7 -1 6 2.45 0.18 -8 -2 6 6.76 0.19 -9 1 6 13.75 0.23 -2 0 5 48.35 0.75 -3 1 5 91.23 1.09 -6 0 6 9.74 0.23 -2 -2 5 2.62 0.28 -7 1 6 3.1 0.16 -5 -1 6 3.63 0.19 -6 -2 6 9.62 0.22 -1 -1 5 90.01 1 1 -1 4 2.35 0.14 -2 0 6 1.95 0.52 0 0 6 2.81 0.54 -1 1 5 74.22 1.68 -3 1 5 61.56 1.45 1 1 5 24.44 1.24 -5 1 5 46.03 0.94 2 0 6 2.1 0.42 3 1 5 15.47 0.74 -7 1 5 16.54 0.61 -1 1 6 4.82 0.58 -2 2 4 9.14 0.14 0 2 4 11.22 0.14 -5 1 6 2.46 0.42 -4 2 4 11.41 0.14 1 1 6 1.97 0.44 2 2 4 1.3 0.12 -2 2 5 1.33 0.51 -7 1 6 2.5 0.33 0 2 5 6.57 0.66 -4 2 5 7.34 0.53 -6 2 4 35.69 0.23 2 2 5 7.99 0.55 -6 2 5 7.7 0.52 -4 0 6 7.56 0.57 -6 0 6 10.44 0.53 -3 1 6 37.61 1.02 -2 2 6 11.12 0.65 -4 2 6 11.02 0.61 0 2 6 13.08 0.65 -6 2 6 6.09 0.43 -11 3 4 16.68 0.23 -10 4 4 8.53 0.18 -8 4 4 7.88 0.2 -7 3 4 38.92 0.34 -12 4 4 32.57 0.27 -13 3 4 53.72 0.34 -10 2 4 1.12 0.16 -8 2 4 14.51 0.23 -12 2 4 143.01 0.56 -6 4 4 18.64 0.26 -5 3 4 13.72 0.24 -9 5 4 13.85 0.2 -6 2 4 30.25 0.31 -15 3 4 22.24 0.23 -14 2 4 62.26 0.38 -9 1 4 73.07 0.42 -11 1 4 74.46 0.41 -7 1 4 76.45 0.47 -4 2 4 8.9 0.22 -3 3 4 19.31 0.29 -5 1 4 23.78 0.32 -11 3 5 14.42 0.6 -9 3 5 -38.28 1.41 -2 2 4 9.23 0.24 -10 2 5 -13.71 0.94 -7 3 5 -0.88 0.48 -8 4 5 24.44 0.93 -12 2 5 24.07 0.88 -8 2 5 -29.44 1.24 -8 0 4 7.99 0.21 -3 1 4 51.96 0.47 -6 4 5 7.02 0.61 -6 2 5 -9.53 0.62 -5 3 5 2.51 0.69 -6 0 4 59.81 0.48 -10 2 3 58.5 0.9 -8 2 3 72.7 0.96 -12 4 3 1.04 0.27 -13 3 3 34.54 0.68 -6 4 3 1.76 0.32 -12 2 3 12.96 0.44 -5 3 3 45.13 0.78 -9 5 3 11.22 0.53 -14 4 3 12.64 0.43 -11 5 3 0.96 0.3 -15 3 3 5.17 0.29 -19 -1 4 6.34 0.13 -16 -2 4 21.5 0.22 -20 0 4 1.62 0.09 -18 -2 4 14.65 0.18 -21 -1 4 7.76 0.11 -15 -3 4 21.92 0.22 -16 0 5 2.46 0.24 -15 -1 5 7.69 0.41 -20 -2 4 1.07 0.08 -17 -3 4 13.11 0.16 -17 -1 5 21.87 0.43 -18 0 5 1.56 0.17 -14 -2 5 15.12 0.52 -16 -2 5 0.82 0.21 -19 -1 5 1.06 0.13 -18 -2 5 2.42 0.18 -20 0 5 12.98 0.17 -23 1 2 5.72 0.15 -23 -1 2 6.38 0.17 -18 -2 3 21.89 0.46 -21 1 3 9.54 0.23 -21 -1 3 9.63 0.25 -22 -2 2 2.01 0.13 -22 0 3 2.49 0.14 -20 -2 3 0.79 0.15 -14 0 5 20.94 0.59 -2 8 1 1.03 0.2 -6 8 -1 0.29 0.09 -4 8 1 1.08 0.17 -9 7 1 0.22 0.18 -6 8 1 2.43 0.07 -9 7 2 0.32 0.18 -2 8 2 1.28 0.16 -4 8 2 0.88 0.13 -1 7 2 16.69 0.59 0 8 1 4.06 0.27 -3 7 2 2.68 0.31 -5 7 2 5.48 0.36 -7 7 2 8.28 0.35 -10 6 2 2.11 0.26 -6 6 3 15.14 0.5 -8 6 3 6.24 0.35 -3 7 3 0.49 0.24 -5 7 3 7.06 0.32 -12 6 2 0.57 0.2 -7 7 3 12.48 0.34 -10 6 3 10.56 0.36 -5 7 0 -2.13 0.42 -2 8 -2 0.29 0.17 -3 7 1 3.32 0.46 -1 7 1 0.68 0.48 -9 7 0 19.27 0.5 -6 8 -1 0.47 0.15 -4 8 0 -0.81 0.26 -10 6 1 0.72 0.29 -7 7 1 1.69 0.31 -6 8 0 2.11 0.21 -9 7 1 0.36 0.23 -2 8 1 0.96 0.26 -4 8 1 1.14 0.22 -7 7 -1 3.36 0.32 0 8 -1 3.67 0.32 -2 8 -1 2.82 0.27 -9 7 -1 11.29 0.35 -4 8 -1 2.91 0.24 -5 7 1 4.24 0.43 -3 7 2 2.16 0.45 -5 7 2 7.44 0.48 -1 7 2 19.91 0.75 -10 6 2 2.98 0.32 -8 6 -4 0.04 0.06 -3 7 -4 0.32 0.04 -7 7 -2 0.25 0.17 -7 7 -1 3.52 0.12 -10 6 0 18.23 0.43 -7 7 0 8.26 0.31 -12 6 0 26.02 0.46 -9 7 0 24.32 0.42 -10 6 1 0.46 0.24 -15 5 0 15.8 0.36 -11 7 0 7.29 0.22 -14 6 0 3.8 0.2 -9 7 1 0.44 0.17 -13 7 0 9.51 0.18 -11 7 1 0.46 0.13 -16 6 0 23.65 0.28 -8 6 -3 0.03 0.19 -3 7 -3 2.3 0.22 -11 5 -3 5.64 0.27 -5 7 -3 0.71 0.15 -5 7 -2 9.74 0.35 -10 6 -3 1.48 0.16 -10 6 -2 4.67 0.26 -7 7 -3 1.15 0.13 -10 6 -1 9.1 0.35 -13 5 -1 11.68 0.36 -9 7 -2 1.95 0.15 -12 6 -2 3.52 0.2 -12 6 -3 6.63 0.16 -12 6 -1 8.25 0.29 -9 7 -1 15.4 0.34 -11 7 -1 11.48 0.25 -14 6 -1 12.55 0.27 -12 6 1 2.45 0.23 -14 6 -2 1.32 0.1 -15 5 1 12.21 0.33 -10 6 2 2.49 0.24 -14 6 1 1.71 0.18 -13 5 2 40.07 0.59 -12 6 2 0.79 0.18 -15 5 2 9.3 0.29 -17 5 1 5.19 0.19 -16 4 2 11.15 0.32 -13 7 1 1.11 0.1 -16 6 1 2.67 0.13 -14 6 2 0.67 0.14 -13 5 3 7.36 0.29 -11 7 2 1.71 0.13 -10 6 3 10.2 0.32 -8 -4 4 8.8 0.12 -4 -4 4 23.48 0.18 -7 -5 4 17.05 0.15 -5 -5 4 12.9 0.15 -5 -3 4 14.71 0.14 -3 -5 4 14.93 0.17 -2 -4 4 7.34 0.15 -3 -3 4 15.6 0.17 -1 -5 4 5.03 0.14 -1 -3 4 1.09 0.11 0 -4 4 44.84 0.27 -4 -2 4 8.92 0.12 -2 -2 4 10.27 0.13 1 -5 4 6.19 0.15 1 -3 4 1.02 0.11 2 -4 4 17.05 0.2 0 -2 4 11.49 0.14 -6 -4 5 11.42 0.41 -4 -4 5 24.85 0.59 -5 -3 5 9.63 0.48 3 -3 4 7.84 0.15 -2 -4 5 3.38 0.46 -3 -3 5 -35.07 0.71 2 -2 4 1.16 0.1 -1 -3 5 15.89 0.73 0 -4 5 -7.49 0.64 -4 -2 5 7.25 0.42 -2 -2 5 -0.93 0.31 1 -1 4 3.83 0.1 1 -3 5 2.7 0.51 4 -2 4 45.33 0.29 2 -4 5 0.59 0.46 0 -2 5 -1.89 0.43 -3 -1 5 -67.48 1.01 3 -3 5 1.65 0.32 3 -1 4 27.77 0.18 2 -2 5 4.06 0.43 -1 -1 5 -16.27 1.02 6 -2 4 4.45 0.12 1 -1 5 -11.85 0.73 5 -1 4 32.48 0.23 4 -2 5 42.3 0.82 5 -3 5 66.59 0.88 2 0 4 69.38 0.26 3 -1 5 6.78 0.53 -2 0 5 3.9 0.79 0 0 5 -22.08 0.92 4 0 4 240.65 0.47 6 -2 5 29.32 0.63 7 -1 4 16.04 0.16 5 -1 5 82.64 1.08 2 0 5 -3.49 0.72 1 -1 6 2.37 0.32 1 1 4 3.1 0.09 4 -2 6 1.45 0.24 6 0 4 3.54 0.11 4 0 5 18.07 1.1 -2 0 6 1.47 0.32 3 1 4 19 0.15 7 -1 5 6.18 0.55 -6 -6 2 15.86 0.52 -8 -6 2 11.05 0.39 -1 -5 2 15.77 0.47 -4 -6 2 8.52 0.43 -10 -6 2 2.46 0.2 -2 -6 2 16.02 0.51 1 -5 2 13.28 0.41 -6 -4 3 1.57 0.27 -8 -4 3 0.75 0.22 -7 -3 3 88.45 0.92 -4 -4 3 14.92 0.48 -5 -3 3 41.46 0.66 -7 -5 3 10.39 0.42 0 -6 2 8.34 0.39 -5 -5 3 3.18 0.33 -9 -5 3 11.85 0.37 -2 -4 3 2.76 0.28 -3 -5 3 5.46 0.38 -6 -6 3 13.47 0.46 -8 -6 3 6.83 0.32 -1 -5 3 13.14 0.48 -4 -6 3 18.34 0.54 0 -4 3 23.3 0.54 -2 -6 3 4.45 0.36 1 -5 3 18.07 0.5 2 -4 3 12.52 0.41 0 -6 3 12.41 0.44 3 -3 3 10.86 0.33 -3 -3 6 30.63 0.62 -1 -3 6 8.69 0.39 -4 -2 6 15.07 0.49 -2 -2 6 17.64 0.55 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0.65 -11 1 3 3.09 0.3 -16 0 3 24.08 0.53 -13 1 2 179.09 1.27 -14 0 3 29.43 0.6 -17 -1 3 20.21 0.47 -12 0 3 2.11 0.27 -16 0 2 44.03 0.63 -18 -2 3 23.93 0.45 -10 0 3 0.73 0.23 -15 -1 3 6.47 0.32 -14 0 2 15.58 0.4 -17 -1 2 7.97 0.3 -17 -3 3 11.27 0.31 -16 -2 3 14.54 0.39 -13 -1 3 32.81 0.58 -12 0 2 58.6 0.67 -18 -2 2 28.61 0.49 -11 -1 3 3.09 0.25 -14 -2 3 36.5 0.58 -15 -1 2 14.9 0.39 -15 -3 3 4.21 0.25 -12 -2 3 10.76 0.34 -14 -4 3 10.65 0.32 -17 -3 2 2.26 0.23 -13 -3 3 27.8 0.51 -13 -1 2 167.39 1.11 -10 -2 3 53.93 0.68 -12 -4 3 0.79 0.21 -16 -4 2 11.44 0.33 -11 -3 3 6.75 0.3 -16 -2 1 6.91 0.28 -17 -3 1 18.9 0.41 -14 -2 2 4.7 0.28 -15 -3 2 2.88 0.26 -13 -1 1 32.1 0.46 -16 -4 1 5.76 0.28 -14 -4 2 11.5 0.35 -12 -2 2 1.41 0.19 -13 -5 2 39.84 0.56 -14 -2 1 12.89 0.35 -13 -3 2 56.5 0.71 -15 -3 1 21.18 0.46 -12 -4 2 17.99 0.43 -11 -5 2 17.72 0.42 -11 -3 2 8.71 0.31 -14 -4 1 15.76 0.43 -12 -2 1 2.98 0.21 -13 -3 1 11.33 0.36 -10 -4 2 21.34 0.46 -9 -3 2 1.69 0.19 -12 -4 1 27.18 0.54 -8 -4 2 34.24 0.56 -11 -3 1 2.21 0.23 -13 -5 -1 13.05 0.41 -11 -5 -2 18.26 0.48 -11 -3 -1 104.5 0.97 -8 -6 -2 1.44 0.23 -9 -5 -2 10.17 0.41 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.4745 4.3048 -0.2712 0.9354 0.2788 0.2174 -1.3231 -0.8727 3.9645 -0.4419 -0.1290 0.8877 -2.4433 -4.3110 0.1063 -0.9261 -0.2761 -0.2571 12.2847 -0.3214 -0.0146 0.3819 -0.9198 0.0899 -12.2847 0.3214 0.0146 -0.3819 0.9198 -0.0899 0.9207 0.1286 -4.0382 0.2880 0.0831 -0.9540 -0.9207 -0.1286 4.0382 -0.2880 -0.0831 0.9540