#------------------------------------------------------------------------------ #$Date: 2023-09-06 04:45:34 +0300 (Wed, 06 Sep 2023) $ #$Revision: 286220 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312283.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_2312283 loop_ _publ_author_name 'Biryukov, Yaroslav P.' 'Zinnatullin, Almaz L.' 'Levashova, Irina O.' 'Shablinskii, Andrey P.' 'Bubnova, Rimma S.' 'Vagizov, Farit G.' 'Ugolkov, Valery L.' 'Filatov, Stanislav K.' 'Pekov, Igor V.' _publ_section_title ; Crystal structure refinement, low- and high-temperature X-ray diffraction and Mössbauer spectroscopy study of the oxoborate ludwigite from the Iten'yurginskoe deposit. ; _journal_coeditor_code RA5133SUP1 _journal_issue 5 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_paper_doi 10.1107/S2052520623006455 _journal_volume 79 _journal_year 2023 _chemical_formula_sum 'Al0.08 B Fe1.183 Mg1.737 O5' _chemical_formula_weight 201.26 _space_group_IT_number 55 _space_group_name_Hall '-P 2 2ab' _space_group_name_H-M_alt 'P b a m' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 55 _symmetry_space_group_name_Hall '-P 2 2ab' _symmetry_space_group_name_H-M 'P b a m' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2532(14) _cell_length_b 12.3025(18) _cell_length_c 3.0256(5) _cell_measurement_reflns_used 436 _cell_measurement_temperature 293 _cell_measurement_theta_max 32.72 _cell_measurement_theta_min 3.98 _cell_volume 344.43(9) _computing_cell_refinement 'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)' _diffrn_ambient_temperature 293 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.9 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_unetI/netI 0.1064 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 2325 _diffrn_reflns_theta_full 31.13 _diffrn_reflns_theta_max 32.98 _diffrn_reflns_theta_min 3.98 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 5.345 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.881 _exptl_crystal_description prism _exptl_crystal_F_000 389 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.40 _refine_diff_density_min -1.64 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_gt 1.72 _refine_ls_goodness_of_fit_ref 1.53 _refine_ls_number_constraints 10 _refine_ls_number_parameters 60 _refine_ls_number_reflns 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0469 _refine_ls_shift/su_max 0.0446 _refine_ls_shift/su_mean 0.0137 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0434 _reflns_number_gt 272 _reflns_number_total 380 _reflns_threshold_expression I>3\s(I) _cod_data_source_file ra5133sup1.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_sg_symbol_Hall '-P -2xab;-2yab;-2z' _cod_database_code 2312283 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z 3 -x+1/2,y+1/2,-z 4 x+1/2,-y+1/2,-z 5 -x,-y,-z 6 x,y,-z 7 x+1/2,-y+1/2,z 8 -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_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe4 Fe 0.73942(19) 0.38552(11) 0.5 Uani 0.0065(5) 4 0.90 d . . . Mg4 Mg 0.73942(19) 0.38552(11) 0.5 Uani 0.0065(5) 4 0.02 d . . . Al4 Al 0.73942(19) 0.38552(11) 0.5 Uani 0.0065(5) 4 0.08 d . . . Mg2 Mg 0.5 0 0.5 Uani 0.0089(9) 2 0.477(18) d . . . Fe2' Fe 0.5 0 0.5 Uani 0.0089(9) 2 0.523(18) d . . . Mg3 Mg 0.0021(4) 0.2796(2) 0 Uani 0.0101(11) 4 0.978(12) d . . . Fe3' Fe 0.0021(4) 0.2796(2) 0 Uani 0.0101(11) 4 0.022(12) d . . . Mg1 Mg 0 0 0 Uani 0.0077(14) 2 1 d . . . O5 O 0.3498(8) 0.2624(5) 0.5 Uani 0.008(2) 4 1 d . . . O3 O 0.6253(7) 0.1418(5) 0.5 Uani 0.011(2) 4 1 d . . . O1 O 0.8499(8) 0.0442(5) 0.5 Uani 0.010(2) 4 1 d . . . O4 O 0.1104(7) 0.1419(5) 0 Uani 0.011(2) 4 1 d . . . O2 O 0.3843(7) 0.0769(5) 0 Uani 0.012(2) 4 1 d . . . B1 B 0.2733(14) 0.3588(8) 0.5 Uani 0.010(3) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Fe4 Fe 0.0051(9) 0.0075(8) 0.0071(8) 0.0021(7) 0 0 Mg4 Mg 0.0051(9) 0.0075(8) 0.0071(8) 0.0021(7) 0 0 Al4 Al 0.0051(9) 0.0075(8) 0.0071(8) 0.0021(7) 0 0 Mg2 Mg 0.0134(19) 0.0055(14) 0.0077(16) -0.0005(12) 0 0 Fe2' Fe 0.0134(19) 0.0055(14) 0.0077(16) -0.0005(12) 0 0 Mg3 Mg 0.012(2) 0.0090(17) 0.0094(19) 0.0011(16) 0 0 Fe3' Fe 0.012(2) 0.0090(17) 0.0094(19) 0.0011(16) 0 0 Mg1 Mg 0.010(3) 0.008(2) 0.005(2) -0.001(2) 0 0 O5 O 0.011(4) 0.009(3) 0.006(4) -0.003(3) 0 0 O3 O 0.008(4) 0.015(3) 0.010(3) -0.004(3) 0 0 O1 O 0.006(4) 0.012(3) 0.012(4) 0.002(3) 0 0 O4 O 0.016(4) 0.007(3) 0.009(4) 0.000(3) 0 0 O2 O 0.014(4) 0.007(3) 0.016(4) 0.003(3) 0 0 B1 B 0.024(8) 0.006(4) 0.001(5) -0.004(5) 0 0 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0645 0.0514 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' B 0.0013 0.0007 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Mg 0.0486 0.0363 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ti 0.2776 0.4457 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O5 Mg4 O4 4_556 . 4_555 98.5(2) ? O5 Mg4 O4 4_556 . 4_556 98.5(2) ? O5 Mg4 O2 4_556 . 4_555 83.0(2) ? O5 Mg4 O2 4_556 . 4_556 83.0(2) ? O4 Mg4 O4 4_555 . 4_556 101.3(2) ? O4 Mg4 O2 4_555 . 4_555 82.5(2) ? O4 Mg4 O2 4_555 . 4_556 175.6(2) ? O4 Mg4 O2 4_556 . 4_555 175.6(2) ? O4 Mg4 O2 4_556 . 4_556 82.5(2) ? O2 Mg4 O2 4_555 . 4_556 93.7(2) ? O3 Mg2 O3 . . 2_655 180 ? O3 Mg2 O2 . . . 84.6(2) ? O3 Mg2 O2 . . 1_556 84.6(2) ? O3 Mg2 O2 . . 2_655 95.4(2) ? O3 Mg2 O2 . . 2_656 95.4(2) ? O3 Mg2 O2 2_655 . . 95.4(2) ? O3 Mg2 O2 2_655 . 1_556 95.4(2) ? O3 Mg2 O2 2_655 . 2_655 84.6(2) ? O3 Mg2 O2 2_655 . 2_656 84.6(2) ? O2 Mg2 O2 . . 1_556 93.29(18) ? O2 Mg2 O2 . . 2_655 86.71(18) ? O2 Mg2 O2 . . 2_656 180 ? O2 Mg2 O2 1_556 . 2_655 180 ? O2 Mg2 O2 1_556 . 2_656 86.71(18) ? O2 Mg2 O2 2_655 . 2_656 93.29(18) ? O3 Fe2' O3 . . 2_655 180 ? O3 Fe2' O2 . . . 84.6(2) ? O3 Fe2' O2 . . 1_556 84.6(2) ? O3 Fe2' O2 . . 2_655 95.4(2) ? O3 Fe2' O2 . . 2_656 95.4(2) ? O3 Fe2' O2 2_655 . . 95.4(2) ? O3 Fe2' O2 2_655 . 1_556 95.4(2) ? O3 Fe2' O2 2_655 . 2_655 84.6(2) ? O3 Fe2' O2 2_655 . 2_656 84.6(2) ? O2 Fe2' O2 . . 1_556 93.29(18) ? O2 Fe2' O2 . . 2_655 86.71(18) ? O2 Fe2' O2 . . 2_656 180 ? O2 Fe2' O2 1_556 . 2_655 180 ? O2 Fe2' O2 1_556 . 2_656 86.71(18) ? O2 Fe2' O2 2_655 . 2_656 93.29(18) ? O4 Mg3 O2 . . 4_455 178.9(3) ? O5 Fe3' O5 4_455 . 4_456 90.4(2) ? O5 Fe3' O3 4_455 . 4_455 87.70(19) ? O5 Fe3' O3 4_455 . 4_456 165.8(3) ? O5 Fe3' O4 4_455 . . 97.4(2) ? O5 Fe3' O2 4_455 . 4_455 81.9(2) ? O5 Fe3' O3 4_456 . 4_455 165.8(3) ? O5 Fe3' O3 4_456 . 4_456 87.70(19) ? O5 Fe3' O4 4_456 . . 97.4(2) ? O5 Fe3' O2 4_456 . 4_455 81.9(2) ? O3 Fe3' O3 4_455 . 4_456 90.7(2) ? O3 Fe3' O4 4_455 . . 96.8(3) ? O3 Fe3' O2 4_455 . 4_455 83.9(2) ? O3 Fe3' O4 4_456 . . 96.8(3) ? O3 Fe3' O2 4_456 . 4_455 83.9(2) ? O4 Fe3' O2 . . 4_455 178.9(3) ? O4 Mg1 O4 . . 2_555 180 ? O5 B1 O3 . . 4_456 120.6(9) ? O5 B1 O1 . . 4_456 118.5(10) ? O3 B1 O1 4_456 . 4_456 121.0(9) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe4 O5 . 4_556 2.087(7) ? Fe4 O1 . 3_656 2.120(7) ? Fe4 O4 . 4_555 1.956(4) ? Fe4 O4 . 4_556 1.956(4) ? Fe4 O2 . 4_555 2.074(5) ? Fe4 O2 . 4_556 2.074(5) ? Mg4 O5 . 4_556 2.087(7) ? Mg4 O1 . 3_656 2.120(7) ? Mg4 O4 . 4_555 1.956(4) ? Mg4 O4 . 4_556 1.956(4) ? Mg4 O2 . 4_555 2.074(5) ? Mg4 O2 . 4_556 2.074(5) ? Al4 O5 . 4_556 2.087(7) ? Al4 O1 . 3_656 2.120(7) ? Al4 O4 . 4_555 1.956(4) ? Al4 O4 . 4_556 1.956(4) ? Al4 O2 . 4_555 2.074(5) ? Al4 O2 . 4_556 2.074(5) ? Mg2 O3 . . 2.095(6) ? Mg2 O3 . 2_655 2.095(6) ? Mg2 O2 . . 2.081(4) ? Mg2 O2 . 1_556 2.081(4) ? Mg2 O2 . 2_655 2.081(4) ? Mg2 O2 . 2_656 2.081(4) ? Fe2' O3 . . 2.095(6) ? Fe2' O3 . 2_655 2.095(6) ? Fe2' O2 . . 2.081(4) ? Fe2' O2 . 1_556 2.081(4) ? Fe2' O2 . 2_655 2.081(4) ? Fe2' O2 . 2_656 2.081(4) ? Mg3 O5 . 4_455 2.131(6) ? Mg3 O5 . 4_456 2.131(6) ? Mg3 O3 . 4_455 2.127(5) ? Mg3 O3 . 4_456 2.127(5) ? Mg3 O4 . . 1.968(7) ? Mg3 O2 . 4_455 2.075(7) ? Fe3' O5 . 4_455 2.131(6) ? Fe3' O5 . 4_456 2.131(6) ? Fe3' O3 . 4_455 2.127(5) ? Fe3' O3 . 4_456 2.127(5) ? Fe3' O4 . . 1.968(7) ? Fe3' O2 . 4_455 2.075(7) ? Mg1 O1 . 1_454 2.124(5) ? Mg1 O1 . 1_455 2.124(5) ? Mg1 O1 . 2_654 2.124(5) ? Mg1 O1 . 2_655 2.124(5) ? Mg1 O4 . . 2.023(6) ? Mg1 O4 . 2_555 2.023(6) ? O5 B1 . . 1.381(13) ? O3 B1 . 4_556 1.369(14) ? O1 B1 . 4_556 1.388(13) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 123.07 133.75 38.21 o 4 0 0 3485.00 3420.15 76.43 o 6 0 0 282.83 286.61 47.77 o 8 0 0 13631.50 13976.80 296.16 o 10 0 0 0.57 66.87 124.20 < 2 1 0 2.20 0.00 19.11 < 3 1 0 1749.84 1872.49 47.77 o 4 1 0 148.80 171.96 28.66 o 5 1 0 194.23 171.96 28.66 o 6 1 0 87.35 47.77 28.66 < 7 1 0 740.21 754.73 38.21 o 8 1 0 561.26 496.78 47.77 o 9 1 0 0.38 28.66 76.43 < 10 1 0 370.96 305.71 85.98 o 11 1 0 489.33 563.66 105.09 o 1 2 0 4535.89 5015.59 105.09 o 2 2 0 76.93 76.43 28.66 < 3 2 0 2268.80 2369.27 47.77 o 4 2 0 350.65 372.59 28.66 o 5 2 0 3986.09 3878.72 76.43 o 6 2 0 2.57 19.11 28.66 < 7 2 0 3044.80 2952.03 66.87 o 8 2 0 174.85 210.18 47.77 o 9 2 0 418.51 429.91 66.87 o 10 2 0 8.36 152.86 124.20 < 11 2 0 194.32 229.28 143.30 < 1 3 0 33.02 57.32 47.77 < 2 3 0 77.75 95.54 38.21 < 3 3 0 50.18 57.32 28.66 < 4 3 0 310.27 305.71 28.66 o 5 3 0 27.94 76.43 38.21 < 6 3 0 161.73 191.07 47.77 o 7 3 0 973.15 945.80 57.32 o 8 3 0 205.31 143.30 57.32 < 9 3 0 253.70 353.48 76.43 o 10 3 0 168.80 200.62 133.75 < 0 4 0 676.36 773.83 38.21 o 1 4 0 821.04 821.60 57.32 o 2 4 0 18448.80 19183.40 343.93 o 3 4 0 91.78 76.43 38.21 < 4 4 0 204.83 238.84 38.21 o 5 4 0 319.02 267.50 38.21 o 6 4 0 14461.80 13117.00 229.28 o 7 4 0 406.21 372.59 66.87 o 8 4 0 103.10 95.54 66.87 < 9 4 0 95.30 124.20 76.43 < 10 4 0 1463.05 1165.53 152.86 o 1 5 0 648.94 620.98 28.66 o 2 5 0 7717.37 8464.41 171.96 o 3 5 0 1754.02 1853.38 66.87 o 4 5 0 202.57 210.18 47.77 o 5 5 0 2801.17 2684.53 66.87 o 6 5 0 1240.97 1222.85 57.32 o 7 5 0 24.53 47.77 47.77 < 8 5 0 2.76 57.32 66.87 < 9 5 0 1149.87 1050.89 85.98 o 10 5 0 335.70 429.91 143.30 < 0 6 0 42.88 47.77 38.21 < 1 6 0 4939.11 5197.11 85.98 o 2 6 0 2674.61 2636.77 76.43 o 3 6 0 1663.70 1633.65 66.87 o 4 6 0 204.48 181.52 38.21 o 5 6 0 953.82 878.92 57.32 o 6 6 0 699.33 630.53 57.32 o 7 6 0 687.79 573.21 66.87 o 8 6 0 1.88 38.21 57.32 < 9 6 0 833.96 754.73 85.98 o 10 6 0 719.33 563.66 143.30 o 1 7 0 685.43 649.64 38.21 o 2 7 0 35.01 19.11 38.21 < 3 7 0 266.94 334.37 38.21 o 4 7 0 206.37 191.07 47.77 o 5 7 0 152.61 171.96 47.77 o 6 7 0 291.52 315.27 76.43 o 7 7 0 65.21 105.09 66.87 < 8 7 0 183.51 181.52 66.87 < 9 7 0 876.26 945.80 85.98 o 0 8 0 10390.40 10747.70 181.52 o 1 8 0 1663.71 1624.10 38.21 o 2 8 0 190.50 181.52 38.21 o 3 8 0 600.92 544.55 57.32 o 4 8 0 4711.31 4289.52 105.09 o 5 8 0 250.08 248.39 47.77 o 6 8 0 44.88 114.64 66.87 < 7 8 0 561.34 611.42 76.43 o 8 8 0 2564.55 2302.39 105.09 o 9 8 0 301.03 401.25 85.98 o 1 9 0 791.53 754.73 47.77 o 2 9 0 311.57 315.27 38.21 o 3 9 0 1613.75 1671.86 66.87 o 4 9 0 155.33 95.54 57.32 < 5 9 0 253.60 315.27 47.77 o 6 9 0 222.40 324.82 57.32 o 7 9 0 1229.28 1203.74 114.64 o 8 9 0 282.99 305.71 105.09 < 0 10 0 673.88 630.53 57.32 o 1 10 0 263.23 257.95 38.21 o 2 10 0 269.61 238.84 38.21 o 3 10 0 1620.31 1452.13 47.77 o 4 10 0 5946.14 5846.75 152.86 o 5 10 0 1507.13 1394.81 66.87 o 6 10 0 3.79 28.66 57.32 < 7 10 0 400.26 382.14 76.43 o 8 10 0 587.94 363.03 210.18 < 1 11 0 28.42 28.66 38.21 < 2 11 0 152.10 181.52 38.21 o 3 11 0 806.09 716.51 47.77 o 4 11 0 163.12 171.96 38.21 o 5 11 0 84.42 171.96 47.77 o 6 11 0 107.32 162.41 57.32 < 7 11 0 18.96 66.87 114.64 < 0 12 0 199.49 219.73 47.77 o 1 12 0 1227.43 1241.96 66.87 o 2 12 0 1766.76 1853.38 66.87 o 3 12 0 958.72 926.69 47.77 o 4 12 0 149.37 171.96 38.21 o 5 12 0 334.83 458.57 38.21 o 6 12 0 681.56 687.85 95.54 o 1 13 0 568.49 640.09 57.32 o 2 13 0 129.75 200.62 47.77 o 3 13 0 46.79 133.75 47.77 < 4 13 0 19.30 28.66 47.77 < 5 13 0 283.39 315.27 47.77 o 0 14 0 616.45 515.89 95.54 o 1 14 0 268.98 257.95 47.77 o 2 14 0 2925.42 3038.01 95.54 o 3 14 0 308.74 410.80 57.32 o 0 0 1 7651.59 7747.89 219.73 o 2 0 1 15470.60 16890.60 219.73 o 4 0 1 1083.47 1098.65 38.21 o 6 0 1 1477.92 1404.37 66.87 o 8 0 1 654.60 630.53 76.43 o 10 0 1 3117.10 3257.75 191.07 o 1 1 1 833.54 840.71 19.11 o 2 1 1 175.32 200.62 28.66 o 3 1 1 4008.49 4079.35 47.77 o 4 1 1 0.50 -9.55 28.66 < 5 1 1 100.68 133.75 28.66 o 6 1 1 102.86 95.54 28.66 o 7 1 1 1174.32 1098.65 38.21 o 8 1 1 427.57 449.02 57.32 o 9 1 1 49.80 124.20 57.32 < 10 1 1 181.96 133.75 85.98 < 0 2 1 1350.82 1423.47 38.21 o 1 2 1 40.63 57.32 19.11 o 2 2 1 1325.63 1356.60 28.66 o 3 2 1 9978.98 10422.90 114.64 o 4 2 1 2962.79 2952.03 57.32 o 5 2 1 5968.26 5541.03 76.43 o 6 2 1 562.32 563.66 38.21 o 7 2 1 259.10 324.82 38.21 o 8 2 1 486.54 515.89 57.32 o 9 2 1 344.98 429.91 57.32 o 10 2 1 154.15 267.50 85.98 o 1 3 1 1061.21 1003.12 28.66 o 2 3 1 929.46 945.80 28.66 o 3 3 1 5488.46 5875.41 66.87 o 4 3 1 122.54 95.54 28.66 o 5 3 1 6819.89 6534.60 95.54 o 6 3 1 8.30 28.66 38.21 < 7 3 1 100.92 162.41 47.77 o 8 3 1 149.54 238.84 47.77 o 9 3 1 1141.70 1232.40 76.43 o 10 3 1 458.91 535.00 76.43 o 0 4 1 2657.52 2627.21 66.87 o 1 4 1 105.88 114.64 19.11 o 2 4 1 2711.41 2789.62 57.32 o 3 4 1 574.26 535.00 28.66 o 4 4 1 8054.92 8034.50 95.54 o 5 4 1 470.52 410.80 28.66 o 6 4 1 1744.64 1624.10 47.77 o 7 4 1 164.07 257.95 47.77 o 8 4 1 1408.00 1480.79 76.43 o 9 4 1 10.50 162.41 66.87 < 10 4 1 208.79 353.48 105.09 o 1 5 1 311.22 286.61 19.11 o 2 5 1 435.71 487.23 28.66 o 3 5 1 111.44 95.54 28.66 o 4 5 1 571.90 544.55 38.21 o 5 5 1 574.03 592.32 38.21 o 6 5 1 2.77 19.11 38.21 < 7 5 1 145.36 114.64 57.32 < 8 5 1 256.83 219.73 85.98 < 9 5 1 874.09 764.28 105.09 o 0 6 1 13.30 19.11 28.66 < 1 6 1 2613.00 2608.11 38.21 o 2 6 1 1944.88 1948.91 47.77 o 3 6 1 2890.41 2722.75 47.77 o 4 6 1 1.14 28.66 28.66 < 5 6 1 775.31 764.28 38.21 o 6 6 1 462.88 506.34 47.77 o 7 6 1 354.58 439.46 57.32 o 8 6 1 26.53 19.11 114.64 < 9 6 1 632.37 611.42 105.09 o 1 7 1 9133.03 9008.96 124.20 o 2 7 1 100.29 76.43 28.66 < 3 7 1 1035.65 1079.55 38.21 o 4 7 1 144.23 171.96 38.21 o 5 7 1 230.17 296.16 38.21 o 6 7 1 151.58 105.09 38.21 < 7 7 1 4189.32 3926.49 85.98 o 8 7 1 229.98 238.84 85.98 < 9 7 1 1013.43 1136.87 152.86 o 0 8 1 4405.26 4404.17 76.43 o 1 8 1 1497.48 1442.58 38.21 o 2 8 1 1733.01 1585.88 57.32 o 3 8 1 368.05 382.14 38.21 o 4 8 1 1320.44 1175.08 47.77 o 5 8 1 325.45 343.93 38.21 o 6 8 1 629.14 678.30 47.77 o 7 8 1 436.17 544.55 76.43 o 8 8 1 1131.65 1098.65 85.98 o 1 9 1 36.98 85.98 28.66 < 2 9 1 529.60 477.67 38.21 o 3 9 1 178.58 210.18 38.21 o 4 9 1 4.25 143.30 38.21 o 5 9 1 27.63 105.09 47.77 < 6 9 1 152.10 171.96 47.77 o 7 9 1 427.96 449.02 76.43 o 8 9 1 2.29 114.64 76.43 < 0 10 1 49.54 38.21 66.87 < 1 10 1 506.33 535.00 28.66 o 2 10 1 181.41 162.41 38.21 o 3 10 1 812.09 783.39 57.32 o 4 10 1 1008.17 974.46 47.77 o 5 10 1 1122.87 1136.87 57.32 o 6 10 1 690.71 783.39 57.32 o 7 10 1 461.74 554.10 76.43 o 1 11 1 1345.64 1385.26 57.32 o 2 11 1 10.78 66.87 38.21 < 3 11 1 1125.05 1117.76 47.77 o 4 11 1 177.45 143.30 57.32 < 5 11 1 2772.39 2722.75 76.43 o 6 11 1 214.75 372.59 57.32 o 0 12 1 339.93 468.12 57.32 o 1 12 1 2213.43 2264.18 66.87 o 2 12 1 1764.58 1834.27 76.43 o 3 12 1 151.19 143.30 38.21 o 4 12 1 0.49 57.32 57.32 < 5 12 1 83.13 114.64 57.32 < 1 13 1 163.36 219.73 38.21 o 2 13 1 1.63 57.32 66.87 < 3 13 1 36.39 143.30 66.87 < 4 13 1 3.79 19.11 66.87 < 0 14 1 1380.98 1499.90 76.43 o 1 14 1 336.43 334.37 38.21 o 0 0 2 37221.90 33809.90 611.42 o 2 0 2 12.62 -28.66 47.77 < 4 0 2 3146.83 3066.68 66.87 o 6 0 2 112.29 114.64 47.77 < 8 0 2 7416.79 8703.24 315.27 o 1 1 2 95.59 105.09 28.66 o 2 1 2 4.44 0.00 28.66 < 3 1 2 651.22 659.19 28.66 o 4 1 2 30.29 57.32 28.66 < 5 1 2 74.17 76.43 38.21 < 6 1 2 43.05 47.77 38.21 < 7 1 2 421.42 506.34 57.32 o 8 1 2 289.97 458.57 76.43 o 9 1 2 0.49 124.20 85.98 < 0 2 2 230.14 229.28 57.32 o 1 2 2 1975.46 1853.38 47.77 o 2 2 2 30.72 -9.55 38.21 < 3 2 2 1304.81 1280.17 47.77 o 4 2 2 205.64 277.05 38.21 o 5 2 2 1854.67 1891.59 57.32 o 6 2 2 3.08 38.21 38.21 < 7 2 2 1522.07 1624.10 66.87 o 8 2 2 104.25 248.39 76.43 o 9 2 2 236.17 477.67 85.98 o 1 3 2 13.80 47.77 28.66 < 2 3 2 45.27 47.77 28.66 < 3 3 2 53.17 85.98 38.21 < 4 3 2 140.46 162.41 47.77 o 5 3 2 21.45 19.11 47.77 < 6 3 2 69.83 114.64 47.77 < 7 3 2 512.78 592.32 57.32 o 8 3 2 106.27 143.30 76.43 < 0 4 2 161.82 191.07 38.21 o 1 4 2 321.40 324.82 28.66 o 2 4 2 8887.34 8846.55 95.54 o 3 4 2 74.25 105.09 28.66 o 4 4 2 49.37 105.09 38.21 < 5 4 2 166.06 85.98 47.77 < 6 4 2 7498.72 7938.96 152.86 o 7 4 2 203.11 171.96 66.87 < 8 4 2 53.55 57.32 66.87 < 1 5 2 398.97 420.35 28.66 o 2 5 2 2217.00 2130.43 38.21 o 3 5 2 674.31 611.42 38.21 o 4 5 2 76.22 143.30 38.21 o 5 5 2 1369.96 1280.17 57.32 o 6 5 2 566.61 592.32 57.32 o 7 5 2 13.13 38.21 66.87 < 8 5 2 3.76 105.09 133.75 < 0 6 2 3.67 38.21 47.77 < 1 6 2 2172.42 2101.77 47.77 o 2 6 2 1296.51 1241.96 38.21 o 3 6 2 857.16 859.82 47.77 o 4 6 2 99.47 133.75 38.21 o 5 6 2 518.62 563.66 57.32 o 6 6 2 393.55 353.48 66.87 o 7 6 2 380.01 496.78 133.75 o 8 6 2 3.68 19.11 133.75 < 1 7 2 308.46 315.27 38.21 o 2 7 2 16.45 38.21 38.21 < 3 7 2 117.99 85.98 38.21 < 4 7 2 99.51 114.64 38.21 o 5 7 2 103.92 133.75 47.77 < 6 7 2 163.58 210.18 57.32 o 7 7 2 52.51 649.64 105.09 o 0 8 2 5440.32 5139.79 105.09 o 1 8 2 822.03 783.39 38.21 o 2 8 2 105.96 143.30 66.87 < 3 8 2 367.59 334.37 47.77 o 4 8 2 2610.08 2598.55 66.87 o 5 8 2 164.22 229.28 57.32 o 6 8 2 23.28 38.21 76.43 < 7 8 2 328.36 468.12 76.43 o 1 9 2 411.80 439.46 47.77 o 2 9 2 123.31 248.39 66.87 o 3 9 2 865.13 907.58 57.32 o 4 9 2 85.42 114.64 57.32 < 5 9 2 140.13 124.20 57.32 < 6 9 2 133.14 248.39 76.43 o 0 10 2 403.84 391.69 57.32 o 1 10 2 152.47 219.73 47.77 o 2 10 2 173.05 286.61 47.77 o 3 10 2 842.49 802.49 85.98 o 4 10 2 3302.97 3276.85 114.64 o 5 10 2 844.40 878.92 57.32 o 1 11 2 17.44 47.77 57.32 < 2 11 2 83.28 191.07 47.77 o 3 11 2 447.24 792.94 152.86 o 4 11 2 101.02 -296.16 171.96 < 0 12 2 107.63 133.75 143.30 < 1 12 2 760.30 668.74 66.87 o 2 12 2 1077.61 1194.19 66.87 o 0 0 3 1575.17 1433.03 105.09 o 2 0 3 3527.66 3467.92 114.64 o 4 0 3 384.94 449.02 152.86 < 6 0 3 531.50 773.83 105.09 o 1 1 3 276.22 219.73 47.77 o 2 1 3 25.60 152.86 57.32 < 3 1 3 943.09 792.94 85.98 o 4 1 3 0.00 -124.20 105.09 < 5 1 3 29.52 9.55 66.87 < 6 1 3 27.19 95.54 66.87 < 0 2 3 375.28 382.14 66.87 o 1 2 3 142.22 124.20 47.77 < 2 2 3 320.01 372.59 47.77 o 3 2 3 1960.25 2034.90 95.54 o 4 2 3 727.96 601.87 105.09 o 5 2 3 1454.74 1757.84 85.98 o 6 2 3 156.26 219.73 76.43 < 1 3 3 489.23 429.91 57.32 o 2 3 3 146.60 238.84 47.77 o 3 3 3 1199.60 1241.96 85.98 o 4 3 3 36.10 -200.62 114.64 < 5 3 3 2004.17 2130.43 76.43 o 0 4 3 1020.57 1003.12 57.32 o 1 4 3 63.48 57.32 38.21 < 2 4 3 829.22 812.05 57.32 o 3 4 3 141.93 257.95 47.77 o 4 4 3 2231.02 2206.86 76.43 o 5 4 3 125.96 143.30 66.87 < 1 5 3 102.08 162.41 47.77 o 2 5 3 82.74 76.43 66.87 < 3 5 3 40.89 95.54 47.77 < 4 5 3 115.63 162.41 47.77 o 0 6 3 2.51 -19.11 57.32 < 1 6 3 650.26 659.19 47.77 o 2 6 3 499.06 506.34 57.32 o 3 6 3 764.20 697.41 95.54 o 4 6 3 4.93 95.54 85.98 < 1 7 3 2373.51 2225.97 66.87 o 2 7 3 19.96 19.11 47.77 < 3 7 3 423.58 506.34 66.87 o 0 8 3 1401.95 1385.26 95.54 o 1 8 3 485.56 468.12 47.77 o loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 ? ? ? ? ? ? ? ? ? ? ? loop_ _twin_refln_datum_id _twin_refln_individual_id _twin_refln_index_h _twin_refln_index_k _twin_refln_index_l _twin_refln_F_squared_calc _twin_refln_F_squared_meas _twin_refln_F_squared_sigma _twin_refln_include_status ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_c_label _jana_atom_site_adp_c_type_symbol _jana_atom_site_adp_c_111 _jana_atom_site_adp_c_112 _jana_atom_site_adp_c_113 _jana_atom_site_adp_c_122 _jana_atom_site_adp_c_123 _jana_atom_site_adp_c_133 _jana_atom_site_adp_c_222 _jana_atom_site_adp_c_223 _jana_atom_site_adp_c_233 _jana_atom_site_adp_c_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_d_label _jana_atom_site_adp_d_type_symbol _jana_atom_site_adp_d_1111 _jana_atom_site_adp_d_1112 _jana_atom_site_adp_d_1113 _jana_atom_site_adp_d_1122 _jana_atom_site_adp_d_1123 _jana_atom_site_adp_d_1133 _jana_atom_site_adp_d_1222 _jana_atom_site_adp_d_1223 _jana_atom_site_adp_d_1233 _jana_atom_site_adp_d_1333 _jana_atom_site_adp_d_2222 _jana_atom_site_adp_d_2223 _jana_atom_site_adp_d_2233 _jana_atom_site_adp_d_2333 _jana_atom_site_adp_d_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_e_label _jana_atom_site_adp_e_type_symbol _jana_atom_site_adp_e_11111 _jana_atom_site_adp_e_11112 _jana_atom_site_adp_e_11113 _jana_atom_site_adp_e_11122 _jana_atom_site_adp_e_11123 _jana_atom_site_adp_e_11133 _jana_atom_site_adp_e_11222 _jana_atom_site_adp_e_11223 _jana_atom_site_adp_e_11233 _jana_atom_site_adp_e_11333 _jana_atom_site_adp_e_12222 _jana_atom_site_adp_e_12223 _jana_atom_site_adp_e_12233 _jana_atom_site_adp_e_12333 _jana_atom_site_adp_e_13333 _jana_atom_site_adp_e_22222 _jana_atom_site_adp_e_22223 _jana_atom_site_adp_e_22233 _jana_atom_site_adp_e_22333 _jana_atom_site_adp_e_23333 _jana_atom_site_adp_e_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_f_label _jana_atom_site_adp_f_type_symbol _jana_atom_site_adp_f_111111 _jana_atom_site_adp_f_111112 _jana_atom_site_adp_f_111113 _jana_atom_site_adp_f_111122 _jana_atom_site_adp_f_111123 _jana_atom_site_adp_f_111133 _jana_atom_site_adp_f_111222 _jana_atom_site_adp_f_111223 _jana_atom_site_adp_f_111233 _jana_atom_site_adp_f_111333 _jana_atom_site_adp_f_112222 _jana_atom_site_adp_f_112223 _jana_atom_site_adp_f_112233 _jana_atom_site_adp_f_112333 _jana_atom_site_adp_f_113333 _jana_atom_site_adp_f_122222 _jana_atom_site_adp_f_122223 _jana_atom_site_adp_f_122233 _jana_atom_site_adp_f_122333 _jana_atom_site_adp_f_123333 _jana_atom_site_adp_f_133333 _jana_atom_site_adp_f_222222 _jana_atom_site_adp_f_222223 _jana_atom_site_adp_f_222233 _jana_atom_site_adp_f_222333 _jana_atom_site_adp_f_223333 _jana_atom_site_adp_f_233333 _jana_atom_site_adp_f_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?