#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 13/05/2013' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full Mineralogical Magazine _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ? # name ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2006). Jana2006. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Al29.2 As18 Fe2.8 H190 O188' _chemical_formula_weight 5492.2 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I2' _symmetry_space_group_name_Hall I2 _symmetry_Int_Tables_number ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 x+1/2,y+1/2,z+1/2 4 -x+1/2,y+1/2,-z+1/2 _cell_length_a 24.576(5) _cell_length_b 7.754(5) _cell_length_c 24.641(5) _cell_angle_alpha 90 _cell_angle_beta 90.190(10) _cell_angle_gamma 90 _cell_volume 4696(3) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.032(19) 1 0 0 0 1 0 0 0 1 2 0.022(11) 0 0 -1 0 -1 0 -1 0 0 3 0.490(11) -1 0 0 0 -1 0 0 0 -1 4 0.456(11) 0 0 1 0 1 0 1 0 0 _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 100 K _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.9416 _exptl_crystal_density_meas 1.98 _exptl_crystal_density_method ? _exptl_crystal_F_000 2555 _exptl_absorpt_coefficient_mu 3.634 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 26950 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 33.16 _diffrn_reflns_theta_full 18.63 _diffrn_measured_fraction_theta_max 0.86 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 12955 _reflns_number_gt 9769 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_gt 0.0745 _refine_ls_R_factor_all 0.0810 _refine_ls_wR_factor_ref 0.0808 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_goodness_of_fit_gt 1.08 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 12955 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_number_constraints 19 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0025000002F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0929 _refine_ls_shift/su_mean 0.0052 _refine_diff_density_max 0.97 _refine_diff_density_min -0.71 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef -16700(1200) _refine_ls_abs_structure_details ; 4792 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0.490(11) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c Al 0.0645 0.0514 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 6.4202 3.0387 1.9002 0.7426 1.5936 31.547199 1.9646 85.0886 1.1151 As 0.0499 2.0058 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.797199 2.531 Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.880501 1.0369 H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038 O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_mutiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As01 As 0.79768(4) 0.18161(15) 0.75058(4) Uani 0.0263(3) 4 1 d . . . As02 As 0 0.50188(19) 0.5 Uani 0.0217(3) 2 1 d . . . As03 As 0.86884(4) 0.98957(15) 0.58781(4) Uani 0.0249(3) 4 1 d . . . As04 As 0.74933(4) 0.82240(15) 0.29770(4) Uani 0.0261(3) 4 1 d . . . As05 As 0.91225(4) 0.01416(15) 0.36875(4) Uani 0.0250(3) 4 1 d . . . Al01 Al 0.93923(9) 0.8635(2) 0.48702(9) Uani 0.0217(6) 4 0.679(16) d . . . Fe01 Fe 0.93923(9) 0.8635(2) 0.48702(9) Uani 0.0217(6) 4 0.321(16) d . . . Al02 Al 0.98726(9) 0.1407(2) 0.56094(9) Uani 0.0245(7) 4 0.612(16) d . . . Fe02 Fe 0.98726(9) 0.1407(2) 0.56094(9) Uani 0.0245(7) 4 0.388(16) d . . . Al03 Al 0.81069(13) 0.1938(4) 0.31509(13) Uani 0.0247(8) 4 1 d . . . Al04 Al 0.68379(14) 0.3181(4) 0.68950(14) Uani 0.0287(9) 4 1 d . . . Al5 Al 0.68489(13) 0.3095(4) 0.81080(13) Uani 0.0252(8) 4 1 d . . . Al06 Al 0.68957(13) 0.1848(4) 0.31609(14) Uani 0.0282(9) 4 1 d . . . Al07 Al 0.87134(14) 0.9300(4) 0.24973(14) Uani 0.0282(9) 4 1 d . . . Al08 Al 0.74938(15) 0.0738(4) 0.62890(14) Uani 0.0283(9) 4 1 d . . . O01 O 0.8435(4) 0.3385(10) 0.7496(4) Uani 0.037(2) 4 1 d . . . O02 O 0.8056(4) 0.0570(10) 0.8048(4) Uani 0.037(3) 4 1 d . . . O03 O 0.7344(3) 0.2697(9) 0.7524(3) Uani 0.027(2) 4 1 d . . . O04 O 0.7993(3) 0.0576(9) 0.6933(3) Uani 0.027(2) 4 1 d . . . O05 O 0.9888(3) 0.3826(9) 0.5551(3) Uani 0.029(2) 4 1 d . . . O06 O 0.4443(3) 0.1214(9) 0.9889(3) Uani 0.027(2) 4 1 d . . . O07 O 0.8765(3) 0.8734(9) 0.5306(3) Uani 0.027(2) 4 1 d . . . O08 O 0.8106(3) 0.1041(11) 0.5836(4) Uani 0.034(2) 4 1 d . . . O09 O 0.6291(3) 0.3530(9) 0.8593(3) Uani 0.029(2) 4 1 d . . . O010 O 0.9195(3) 0.1353(9) 0.5964(3) Uani 0.028(2) 4 1 d . . . O011 O 0.6952(4) 0.9449(10) 0.3060(4) Uani 0.033(2) 4 1 d . . . O012 O 0.7495(4) 0.1654(10) 0.1568(4) Uani 0.039(3) 4 1 d . . . O013 O 0.7526(3) 0.2322(9) 0.2648(3) Uani 0.027(2) 4 1 d . . . O014 O 0.8071(3) 0.9459(8) 0.2998(3) Uani 0.0249(19) 4 1 d . . . O015 O 0.9162(3) 0.8997(10) 0.3109(4) Uani 0.033(2) 4 1 d . . . O016 O 0.9695(3) 0.1293(9) 0.3766(3) Uani 0.028(2) 4 1 d . . . O017 O 0.8588(3) 0.1500(9) 0.3705(3) Uani 0.031(2) 4 1 d . . . O018 O 0.9037(3) 0.8692(9) 0.4202(3) Uani 0.028(2) 4 1 d . . . O019 O 0.9502(3) 0.1155(8) 0.4891(3) Uani 0.0239(19) 4 1 d . . . O020 O 0.9889(3) 0.8877(8) 0.5500(3) Uani 0.0218(18) 4 1 d . . . O021 O 0.7504(3) 0.1977(10) 0.3609(3) Uani 0.028(2) 4 1 d . . . O022 O 0.8630(3) 0.1663(10) 0.2603(3) Uani 0.029(2) 4 1 d . . . O023 O 0.8260(4) 0.4357(9) 0.3212(3) Uani 0.032(2) 4 1 d . . . O024 O 0.6389(3) 0.3064(10) 0.7504(3) Uani 0.029(2) 4 1 d . . . O025 O 0.6846(3) 0.0851(10) 0.6707(3) Uani 0.032(2) 4 1 d . . . O026 O 0.7398(3) 0.3130(10) 0.6378(3) Uani 0.033(2) 4 1 d . . . O027 O 0.3751(4) 0.3638(13) 0.3600(4) Uani 0.045(3) 4 1 d . . . O028 O 0.7397(3) 0.3372(10) 0.8621(3) Uani 0.028(2) 4 1 d . . . O029 O 0.6782(3) 0.0680(9) 0.8258(3) Uani 0.029(2) 4 1 d . . . O030 O 0.6392(4) 0.1419(14) 0.3739(4) Uani 0.047(3) 4 1 d . . . O031 O 0.8285(4) 0.9184(9) 0.1851(4) Uani 0.032(2) 4 1 d . . . O032 O 0.6378(3) 0.1906(10) 0.2592(3) Uani 0.030(2) 4 1 d . . . O033 O 0.9360(4) 0.9495(11) 0.2070(4) Uani 0.039(3) 4 1 d . . . O034 O 0.7066(4) 0.0567(12) 0.5652(4) Uani 0.040(3) 4 1 d . . . Ow01 O 0.7537(10) 0.575(3) 0.5494(10) Uiso 0.127(8) 4 1 d . . . Ow02 O 0.0590(5) 0.262(2) 0.3009(5) Uiso 0.051(4) 4 0.79(4) d . . . Ow03 O 0.6897(16) 0.437(6) 0.4620(17) Uiso 0.222(17) 4 1 d . . . Ow04 O 0.8561(5) 0.2970(17) 0.4726(5) Uiso 0.059(3) 4 1 d . . . Ow05 O 0.0257(5) 0.7097(17) 0.3540(5) Uiso 0.058(3) 4 1 d . . . Ow06 O 0.6256(5) 0.976(2) 0.9140(5) Uiso 0.063(3) 4 1 d . . . Owo7 O 0.7539(10) 0.061(3) 0.4649(10) Uiso 0.113(7) 4 0.87(5) d . . . Ow08 O 0.9148(4) 0.5260(18) 0.3746(4) Uiso 0.057(2) 4 1 d . . . Ow9 O 0.9876(4) 0.4232(12) 0.3414(4) Uiso 0.0385(18) 4 1 d . . . Ow10 O 0.6602(4) 0.0783(13) 0.9864(4) Uiso 0.042(2) 4 1 d . . . Ow11 O 0.6984(5) 0.244(2) 0.0598(5) Uiso 0.043(4) 4 0.71(4) d . . . Ow12 O 0.9490(9) 0.431(3) 0.2495(9) Uiso 0.088(9) 4 0.78(5) d . . . Ow13 O 0.0333(9) 0.941(3) 0.2586(9) Uiso 0.119(7) 4 1 d . . . Ow14 O 0.6584(18) 0.801(7) 0.4074(18) Uiso 0.057(16) 4 0.25(4) d . . . Ow15 O 0.4078(19) 0.743(7) 0.3461(19) Uiso 0.17(3) 4 0.66(8) 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 As01 As 0.0318(5) 0.0112(4) 0.0359(5) 0.0011(3) 0.0080(4) -0.0008(3) As02 As 0.0270(6) 0.0101(5) 0.0282(6) 0 -0.0001(4) 0 As03 As 0.0320(5) 0.0106(4) 0.0321(5) 0.0003(3) 0.0086(3) 0.0002(3) As04 As 0.0343(5) 0.0108(4) 0.0332(5) -0.0009(3) -0.0069(4) -0.0009(3) As05 As 0.0311(5) 0.0100(4) 0.0339(5) 0.0003(3) -0.0077(3) -0.0004(3) Al01 Al 0.0279(12) 0.0102(9) 0.0270(12) 0.0013(7) 0.0008(7) 0.0005(7) Fe01 Fe 0.0279(12) 0.0102(9) 0.0270(12) 0.0013(7) 0.0008(7) 0.0005(7) Al02 Al 0.0295(12) 0.0105(9) 0.0334(13) -0.0004(6) 0.0000(7) 0.0002(7) Fe02 Fe 0.0295(12) 0.0105(9) 0.0334(13) -0.0004(6) 0.0000(7) 0.0002(7) Al03 Al 0.0330(15) 0.0109(12) 0.0303(15) 0.0025(10) -0.0097(11) -0.0016(10) Al04 Al 0.0371(16) 0.0145(12) 0.0346(16) 0.0022(11) 0.0073(12) -0.0031(12) Al5 Al 0.0304(15) 0.0122(12) 0.0332(16) -0.0011(10) 0.0087(11) -0.0026(10) Al06 Al 0.0330(16) 0.0131(12) 0.0384(16) 0.0032(11) -0.0081(11) 0.0026(11) Al07 Al 0.0351(18) 0.0135(13) 0.0359(18) -0.0002(11) -0.0070(13) -0.0059(11) Al08 Al 0.0370(18) 0.0126(12) 0.0354(18) 0.0034(11) 0.0083(13) -0.0005(11) O01 O 0.052(5) 0.012(3) 0.048(5) -0.003(3) 0.022(4) -0.005(3) O02 O 0.047(5) 0.014(3) 0.049(5) -0.001(3) -0.004(4) -0.001(3) O03 O 0.036(4) 0.014(3) 0.031(4) 0.001(3) 0.007(3) -0.001(2) O04 O 0.027(4) 0.014(3) 0.039(4) 0.003(2) 0.008(3) 0.007(3) O05 O 0.043(4) 0.015(3) 0.030(4) 0.002(3) 0.000(3) -0.005(2) O06 O 0.021(3) 0.017(3) 0.044(4) -0.003(2) 0.003(2) -0.003(3) O07 O 0.035(4) 0.014(3) 0.033(4) 0.000(2) 0.004(3) -0.003(2) O08 O 0.035(4) 0.025(4) 0.042(4) 0.006(3) 0.013(3) 0.007(3) O09 O 0.036(4) 0.016(3) 0.033(4) -0.007(3) 0.011(3) 0.002(2) O010 O 0.040(4) 0.015(3) 0.029(3) -0.004(3) 0.005(3) -0.003(2) O011 O 0.035(4) 0.013(3) 0.051(5) -0.005(3) -0.002(3) -0.002(3) O012 O 0.053(5) 0.012(3) 0.052(5) 0.006(3) -0.020(4) -0.001(3) O013 O 0.034(4) 0.010(3) 0.037(4) 0.001(2) -0.010(3) 0.002(3) O014 O 0.031(4) 0.009(3) 0.034(4) 0.004(2) -0.005(3) -0.003(2) O015 O 0.031(4) 0.023(3) 0.044(4) 0.008(3) -0.008(3) -0.005(3) O016 O 0.032(4) 0.017(3) 0.035(4) -0.003(3) -0.005(3) 0.001(3) O017 O 0.040(4) 0.014(3) 0.037(4) 0.004(3) -0.009(3) -0.002(3) O018 O 0.024(3) 0.017(3) 0.044(4) -0.001(2) -0.012(3) 0.001(3) O019 O 0.028(4) 0.011(3) 0.033(4) 0.001(2) -0.007(2) -0.002(2) O020 O 0.026(3) 0.011(2) 0.028(3) -0.004(2) 0.002(2) 0.001(2) O021 O 0.028(3) 0.025(4) 0.031(4) 0.000(3) -0.007(2) -0.004(3) O022 O 0.040(4) 0.016(3) 0.031(4) 0.003(3) -0.002(3) 0.000(3) O023 O 0.046(5) 0.013(3) 0.037(4) 0.003(3) -0.009(3) -0.001(3) O024 O 0.033(4) 0.019(3) 0.034(4) 0.001(3) 0.010(3) 0.000(3) O025 O 0.035(4) 0.022(4) 0.038(4) 0.007(3) 0.004(3) -0.003(3) O026 O 0.044(4) 0.015(3) 0.039(4) 0.007(3) 0.009(3) 0.008(3) O027 O 0.043(5) 0.036(5) 0.056(6) 0.000(4) -0.012(4) 0.011(4) O028 O 0.037(4) 0.013(3) 0.035(4) -0.008(3) 0.007(3) 0.000(3) O029 O 0.034(4) 0.015(3) 0.038(4) -0.002(2) 0.013(3) -0.004(3) O030 O 0.048(5) 0.046(6) 0.046(5) 0.007(4) -0.002(4) 0.000(4) O031 O 0.044(5) 0.011(3) 0.041(4) -0.004(3) -0.006(3) -0.003(3) O032 O 0.034(4) 0.016(3) 0.040(4) -0.004(3) -0.007(3) 0.002(3) O033 O 0.038(5) 0.034(4) 0.043(5) 0.002(3) 0.001(3) -0.001(3) O034 O 0.040(5) 0.036(5) 0.045(5) 0.001(3) -0.004(3) -0.003(4) 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 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 10. MOLECULAR GEOMETRY 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 As01 O01 . . 1.659(8) ? As01 O02 . . 1.659(9) ? As01 O03 . . 1.699(7) ? As01 O04 . . 1.709(8) ? As02 O05 . 1_455 1.666(7) ? As02 O05 . 2_656 1.666(7) ? As02 O06 . 3_454 1.675(7) ? As02 O06 . 4_556 1.675(7) ? As03 O07 . . 1.685(7) ? As03 O08 . 1_565 1.687(8) ? As03 O09 . 4_656 1.679(7) ? As03 O010 . 1_565 1.695(8) ? As04 O011 . . 1.647(8) ? As04 O012 . 4_655 1.656(8) ? As04 O013 . 4_655 1.692(7) ? As04 O014 . . 1.713(7) ? As05 O015 . 1_545 1.681(9) ? As05 O016 . . 1.678(8) ? As05 O017 . . 1.685(8) ? As05 O018 . 1_545 1.707(8) ? Al01 Fe01 . . 0 ? Al01 O06 . 3_554 1.882(7) ? Al01 O07 . . 1.882(8) ? Al01 O018 . . 1.862(8) ? Al01 O019 . 1_565 1.973(7) ? Al01 O020 . . 1.982(7) ? Al01 O020 . 2_756 1.999(7) ? Fe01 O06 . 3_554 1.882(7) ? Fe01 O07 . . 1.882(8) ? Fe01 O018 . . 1.862(8) ? Fe01 O019 . 1_565 1.973(7) ? Fe01 O020 . . 1.982(7) ? Fe01 O020 . 2_756 1.999(7) ? Al02 Fe02 . . 0 ? Al02 O05 . . 1.881(7) ? Al02 O010 . . 1.883(8) ? Al02 O016 . 2_756 1.869(8) ? Al02 O019 . . 1.997(7) ? Al02 O019 . 2_756 1.984(7) ? Al02 O020 . 1_545 1.981(6) ? Fe02 O05 . . 1.881(7) ? Fe02 O010 . . 1.883(8) ? Fe02 O016 . 2_756 1.869(8) ? Fe02 O019 . . 1.997(7) ? Fe02 O019 . 2_756 1.984(7) ? Fe02 O020 . 1_545 1.981(6) ? Al03 O013 . . 1.911(8) ? Al03 O014 . 1_545 1.961(7) ? Al03 O017 . . 1.835(8) ? Al03 O021 . . 1.865(8) ? Al03 O022 . . 1.879(8) ? Al03 O023 . . 1.919(8) ? Al04 O02 . 4_656 1.876(9) ? Al04 O03 . . 2.020(8) ? Al04 O024 . . 1.867(8) ? Al04 O025 . . 1.865(8) ? Al04 O026 . . 1.879(9) ? Al04 O027 . 2_656 1.924(10) ? Al5 O03 . . 1.912(8) ? Al5 O04 . 4_656 1.965(7) ? Al5 O09 . . 1.853(8) ? Al5 O024 . . 1.868(8) ? Al5 O028 . . 1.857(8) ? Al5 O029 . . 1.916(8) ? Al06 O011 . 1_545 1.882(8) ? Al06 O013 . . 2.035(8) ? Al06 O021 . . 1.858(8) ? Al06 O030 . . 1.918(10) ? Al06 O031 . 4_645 1.865(8) ? Al06 O032 . . 1.891(9) ? Al07 O014 . . 2.010(9) ? Al07 O015 . . 1.881(9) ? Al07 O022 . 1_565 1.863(9) ? Al07 O031 . . 1.909(9) ? Al07 O032 . 4_655 1.882(8) ? Al07 O033 . . 1.914(10) ? Al08 O04 . . 2.006(9) ? Al08 O08 . . 1.892(9) ? Al08 O025 . . 1.901(9) ? Al08 O026 . . 1.882(8) ? Al08 O028 . 4_646 1.867(8) ? Al08 O034 . . 1.892(10) ? O03 O024 . . 2.365(10) ? O04 O028 . 4_646 2.386(11) ? O07 Ow10 . 4_656 2.494(12) ? O013 O021 . . 2.383(10) ? O014 O022 . 1_565 2.401(11) ? O016 Ow9 . . 2.479(12) ? O025 O026 . . 2.372(11) ? O031 O032 . 4_655 2.384(11) ? Ow01 Ow10 . 4_656 2.30(3) ? Ow02 Ow9 . 1_455 2.378(17) ? Ow04 Ow10 . 4_656 2.437(16) ? Ow05 Ow9 . 1_455 2.431(16) ? Ow06 Ow10 . 1_565 2.126(16) ? Ow08 Ow9 . . 2.124(15) ? Ow9 Ow12 . . 2.45(2) ? Ow10 Ow11 . 1_556 2.407(17) ? 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 ? ? ? ? ? ? ? ? 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_ _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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 11. STRUCTURE-FACTOR LIST 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 4 0 0 11591.50 8383.92 464.57 o 6 0 0 1747.75 1533.37 142.54 o 8 0 0 15572.30 14634.40 810.32 o 10 0 0 447.51 631.51 110.78 o 12 0 0 12694.90 8622.56 482.84 o 14 0 0 750.57 825.20 78.23 o 3 -1 0 56886.50 43828.80 2399.27 o 5 -1 0 56800.90 46920.80 2107.07 o 7 -1 0 17120.30 14900.40 690.90 o 9 -1 0 7238.67 5918.17 394.83 o 11 -1 0 6088.15 6670.91 417.36 o 13 -1 0 5396.30 5250.20 350.62 o 15 -1 0 11443.10 11171.20 641.59 o 17 -1 0 26526.50 24243.00 1341.34 o 19 -1 0 30438.70 28889.00 1594.14 o 21 -1 0 561.25 388.14 150.07 < 23 -1 0 2413.85 2599.25 170.07 o 0 2 0 10107.60 11667.70 954.34 o 0 -2 0 10081.80 10104.50 911.72 o 2 2 0 102601.00 85626.60 6622.90 o 2 -2 0 95683.20 86841.20 6722.47 o 4 2 0 65219.30 57954.90 4415.06 o 4 -2 0 57216.50 55995.20 2526.86 o 6 -2 0 7162.15 10359.80 444.24 o 8 -2 0 23611.10 31259.70 1222.97 o 10 -2 0 36630.30 34776.40 1355.95 o 12 -2 0 5706.19 7899.16 338.00 o 14 -2 0 15356.10 15372.50 878.90 o 16 -2 0 8119.93 9358.11 574.74 o 18 -2 0 7817.59 7889.66 498.96 o 20 -2 0 10588.10 9574.23 581.25 o 22 -2 0 12939.70 14466.00 833.27 o 24 -2 0 7661.61 8145.82 512.44 o 26 -2 0 966.49 573.24 172.26 o 1 -3 0 18450.60 20883.80 845.62 o 3 -3 0 11468.80 15743.80 649.53 o 5 -3 0 90255.70 77508.10 3003.32 o 7 -3 0 4061.72 4555.10 256.15 o 9 -3 0 6004.94 5157.37 271.59 o 11 -3 0 11957.70 12537.20 519.92 o 13 -3 0 1939.74 998.76 156.13 o 15 -3 0 9513.67 9584.99 410.20 o 17 -3 0 9446.88 9928.80 624.95 o 19 -3 0 4955.71 5008.38 390.01 o 21 -3 0 1567.25 1639.08 293.79 o 23 -3 0 3999.21 5112.42 396.93 o 25 -3 0 266.37 187.68 271.97 < 27 -3 0 1092.03 1573.72 277.92 o 29 -3 0 1381.76 1524.26 235.95 o 0 -4 0 8421.91 13614.20 817.15 o 2 -4 0 16919.00 17373.60 716.46 o 4 -4 0 17389.00 17933.50 733.71 o 6 -4 0 37737.00 34668.50 1364.54 o 8 -4 0 7153.13 7541.07 358.11 o 10 -4 0 32983.00 31806.80 1254.75 o 12 -4 0 45154.90 37743.90 1479.30 o 14 -4 0 19238.20 15121.00 621.71 o 16 -4 0 1457.39 1632.06 186.92 o 18 -4 0 1893.37 1744.67 167.21 o 20 -4 0 1147.57 1069.14 287.41 o 22 -4 0 7347.01 5809.59 453.36 o 24 -4 0 3664.55 3751.79 359.52 o 26 -4 0 990.31 1698.01 335.41 o 28 -4 0 1674.01 1509.29 314.18 o 30 -4 0 3626.62 3157.28 354.20 o 32 -4 0 1621.48 1230.13 228.88 o 1 -5 0 757.83 537.46 222.25 < 3 -5 0 44812.80 44263.30 1736.20 o 5 -5 0 11208.20 9803.65 455.07 o 7 -5 0 16409.80 16061.50 669.54 o 9 -5 0 2207.21 2555.76 293.60 o 11 -5 0 1109.73 1363.40 226.78 o 13 -5 0 3820.44 3660.50 273.11 o 15 -5 0 1270.17 785.17 246.71 o 17 -5 0 5545.17 5589.40 294.06 o 19 -5 0 6905.75 6324.64 378.85 o 21 -5 0 1589.74 1734.63 221.81 o 23 -5 0 336.98 439.08 364.34 < 25 -5 0 408.46 446.12 360.39 < 27 -5 0 2287.67 2492.01 358.31 o 29 -5 0 444.81 661.81 296.86 < 31 -5 0 202.39 156.54 322.01 < 0 -6 0 93177.40 91068.30 7054.95 o 2 -6 0 2159.97 2320.58 257.98 o 4 -6 0 360.22 905.28 246.61 o 6 -6 0 4988.52 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356.90 o -9 -5 30 831.99 860.36 321.86 < -7 5 30 541.66 354.81 340.07 < -7 -5 30 449.59 35.29 317.45 < -5 5 30 1441.50 664.21 430.91 < -5 -5 30 1460.93 1047.15 245.55 o -3 5 30 616.50 -298.52 441.77 < -3 -5 30 634.15 645.21 246.21 < -1 5 30 255.77 -80.96 399.63 < -1 -5 30 350.27 59.78 219.83 < 1 5 30 261.07 -266.58 425.61 < 1 -5 30 348.65 67.89 230.66 < 3 5 30 590.21 457.49 429.89 < 3 -5 30 604.82 1045.32 222.10 o 5 5 30 1453.73 1356.37 422.87 o 5 -5 30 1494.63 1434.80 240.07 o 7 5 30 470.61 694.52 420.33 < 7 -5 30 404.86 349.35 275.87 < 9 5 30 948.48 -767.56 800.57 < 9 -5 30 829.38 593.99 307.07 < 11 5 30 527.41 303.87 857.66 < 11 -5 30 458.45 263.00 319.46 < 13 5 30 160.44 352.75 795.81 < 13 -5 30 188.44 284.85 366.65 < 15 5 30 1120.55 -99.61 601.78 < 15 -5 30 1318.31 1938.51 441.52 o -19 0 31 188.48 -362.70 341.52 < -17 0 31 1547.41 2186.07 361.99 o -15 0 31 55.79 -401.95 302.92 < -13 0 31 270.58 106.91 347.71 < -11 0 31 1628.65 1475.66 387.59 o -9 0 31 1003.25 1215.83 377.04 o -7 0 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3872.88 422.28 o 5 0 33 812.56 2078.95 612.49 o 7 0 33 1473.12 1136.55 333.89 o 9 0 33 1270.84 1624.08 336.19 o 11 0 33 110.28 254.54 324.30 < 13 0 33 118.88 401.74 343.20 < 15 0 33 461.94 -311.14 357.64 < 17 0 33 142.20 -660.45 406.11 < -12 1 33 1195.25 1413.36 335.69 o -10 1 33 136.60 -483.74 329.48 < -10 -1 33 135.44 77.86 285.48 < -8 1 33 341.25 346.90 340.25 < -8 -1 33 261.09 438.88 324.49 < -6 1 33 865.04 622.38 387.87 < -6 -1 33 812.33 477.09 293.85 < -4 1 33 911.76 644.70 387.19 < -4 -1 33 802.63 455.71 348.84 < -2 1 33 554.93 592.35 408.25 < -2 -1 33 555.95 962.02 354.50 < 0 1 33 879.17 1331.52 406.00 o 0 -1 33 803.55 682.70 333.77 < 2 1 33 537.46 100.28 353.99 < 2 -1 33 533.57 81.80 314.33 < 4 1 33 909.82 967.93 366.66 < 4 -1 33 820.18 570.54 332.40 < 6 1 33 861.81 785.76 361.22 < 6 -1 33 775.79 558.48 331.14 < 8 1 33 342.85 175.84 322.61 < 8 -1 33 264.78 -457.98 511.13 < 10 1 33 155.71 89.28 341.74 < 10 -1 33 136.08 -33.43 285.48 < 12 1 33 1151.39 1220.44 348.58 o 12 -1 33 1097.88 1182.76 336.57 o 14 1 33 128.96 633.23 345.68 < 14 -1 33 116.49 648.60 386.38 < 16 -1 33 268.03 102.98 432.27 < 18 -1 33 162.99 -441.18 379.52 < -11 2 33 393.37 144.27 340.23 < -9 2 33 101.76 197.24 328.87 < -9 -2 33 73.29 145.13 287.97 < -7 2 33 1210.42 445.62 376.12 < -7 -2 33 1025.59 1015.91 311.25 o -5 2 33 16.09 137.24 383.90 < -5 -2 33 43.01 -88.03 308.32 < -3 2 33 403.34 -156.51 383.39 < -3 -2 33 382.89 670.69 320.50 < -1 2 33 1819.64 1101.75 397.90 < -1 -2 33 1980.81 1548.24 544.65 < 1 2 33 1742.22 1456.67 355.77 o 1 -2 33 1892.08 1747.27 334.98 o 3 2 33 398.25 393.85 367.69 < 3 -2 33 378.70 313.71 308.52 < 5 2 33 21.73 193.51 359.61 < 5 -2 33 50.34 293.99 305.20 < 7 2 33 1142.45 -190.60 333.02 < 7 -2 33 945.37 1029.35 303.33 o 9 2 33 95.84 38.41 295.02 < 9 -2 33 75.89 -475.87 284.23 < 11 2 33 363.05 862.25 344.65 < 11 -2 33 334.88 213.02 389.50 < 13 2 33 523.65 1122.18 649.94 < 13 -2 33 488.90 598.67 366.59 < 15 -2 33 725.52 311.99 370.11 < 17 -2 33 481.73 375.89 386.68 < -6 3 33 433.97 1022.60 343.36 < -4 3 33 439.33 335.31 338.84 < -4 -3 33 352.85 669.59 332.41 < -2 3 33 1464.72 1176.54 346.82 o -2 -3 33 1262.77 1476.06 335.04 o 0 3 33 210.29 -141.80 360.41 < 0 -3 33 221.05 210.51 315.36 < 2 3 33 1499.86 1229.28 340.28 o 2 -3 33 1264.06 1262.52 340.91 o 4 3 33 402.69 -192.00 346.02 < 4 -3 33 319.92 657.62 299.12 < 6 3 33 473.63 261.36 332.15 < 6 -3 33 485.95 695.03 311.81 < 8 3 33 455.56 111.49 546.01 < 8 -3 33 433.74 761.72 363.73 < 10 -3 33 951.34 1286.70 397.07 o 12 -3 33 365.69 770.05 363.54 < -6 0 34 522.64 1196.24 353.14 o -4 0 34 163.82 374.55 333.02 < -2 0 34 269.13 264.51 335.94 < 0 0 34 153.59 25.54 290.87 < 2 0 34 237.86 78.47 336.09 < 4 0 34 202.78 -93.01 295.42 < 6 0 34 550.07 806.17 269.83 < 8 0 34 3457.29 2826.96 341.52 o 10 0 34 241.02 446.17 338.83 < 12 0 34 35.13 -57.51 375.18 < -7 1 34 840.62 1100.07 349.39 o -5 1 34 239.45 147.00 341.75 < -5 -1 34 263.77 314.96 330.54 < -3 1 34 445.49 -33.21 376.52 < -3 -1 34 415.84 305.96 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