#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/39/2013918.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_2013918 loop_ _publ_author_name 'Redhammer, G\"unther J.' 'Roth, G.' _publ_section_title ; The ferri-annite KFe^2+^~3~(Al~0.26~Fe^3+^~0.76~Si~3~)O~10~(OH)~2~ at 100 and 270 K ; _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first i33 _journal_page_last i36 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'K Fe3 (Al0.26 Fe0.76 Si3) O10 (O H)2' _chemical_formula_moiety 'K , Fe3 Al0.24 Fe0.74 Si3 , O10 , 2 OH' _chemical_formula_sum 'Al0.24 Fe3.76 H2 K O12 Si3' _chemical_formula_weight 533.82 _chemical_name_common 'trioctahedral mica' _chemical_name_systematic 'potassium triiron(II) aluminasilaferrate(III) decaoxide dihydroxide' _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 100.06(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.4208(14) _cell_length_b 9.3881(17) _cell_length_c 10.330(3) _cell_measurement_reflns_used 3729 _cell_measurement_temperature 270.0(10) _cell_measurement_theta_max 32.30 _cell_measurement_theta_min 2.1 _cell_volume 517.6(2) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction X-AREA _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 270.0(10) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'Stoe IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3927 _diffrn_reflns_theta_full 32.11 _diffrn_reflns_theta_max 32.11 _diffrn_reflns_theta_min 2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.003 _exptl_absorpt_correction_T_max 0.52 _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'via equivalents (X-SHAPE and X-RED; Stoe & Cie 1996)' _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 3.425 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description cuboid _exptl_crystal_F_000 519.7 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.397 _refine_diff_density_min -0.498 _refine_ls_extinction_coef 0.0147(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 938 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_gt 0.0195 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0486 _reflns_number_gt 814 _reflns_number_total 938 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bc1034.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/m' _[local]_cod_chemical_formula_sum_orig 'Al0.24 Fe3.76 H2 K1 O12 Si3' _cod_database_code 2013918 loop_ _symmetry_equiv_pos_as_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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 0.5 0.0 0.5 0.01006(10) Uani d S 1 . . Fe Fe2 1.0 0.16817(2) 0.5 0.01007(9) Uani d S 1 . . Fe Si 0.57484(6) 0.16659(3) 0.22450(3) 0.01201(12) Uani d P 0.75 . . Si Fe3 0.57484(6) 0.16659(3) 0.22450(3) 0.01201(12) Uani d P 0.189(2) . . Fe Al 0.57484(6) 0.16659(3) 0.22450(3) 0.01201(12) Uani d P 0.061(3) . . Al K 0.0 0.0 0.0 0.0370(2) Uani d S 1 . . K O1 0.8231(2) 0.23295(15) 0.16838(11) 0.0321(3) Uani d . 1 . . O O2 0.5218(4) 0.0 0.16822(16) 0.0322(4) Uani d S 1 . . O O3 0.62963(18) 0.16651(9) 0.38925(10) 0.01202(19) Uani d . 1 . . O O4 0.1309(2) 0.0 0.39564(13) 0.0121(2) Uani d S 1 . . O H 0.106(6) 0.0 0.310(4) 0.035(8) Uiso d S 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.00842(17) 0.00838(17) 0.01370(17) 0.0 0.00281(12) 0.0 Fe2 0.00802(14) 0.00859(14) 0.01370(14) 0.0 0.00221(9) 0.0 Si 0.01165(17) 0.01229(17) 0.01221(17) -0.00003(11) 0.00236(11) -0.00012(11) Fe3 0.01165(17) 0.01229(17) 0.01221(17) -0.00003(11) 0.00236(11) -0.00012(11) Al 0.01165(17) 0.01229(17) 0.01221(17) -0.00003(11) 0.00236(11) -0.00012(11) K 0.0432(5) 0.0448(5) 0.0225(3) 0.0 0.0040(3) 0.0 O1 0.0334(7) 0.0431(8) 0.0198(5) -0.0082(5) 0.0053(4) -0.0017(5) O2 0.0466(11) 0.0298(9) 0.0186(7) 0.0 0.0012(7) 0.0 O3 0.0104(4) 0.0114(4) 0.0147(4) 0.0001(3) 0.0035(3) 0.0002(3) O4 0.0115(6) 0.0129(6) 0.0119(6) 0.0 0.0022(4) 0.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 O4 . 2.1004(14) yes Fe1 O3 5_656 2.1277(9) yes Fe2 O4 5_656 2.1037(9) yes Fe2 O3 8 2.1195(10) yes Fe2 O3 . 2.1301(11) yes Si O2 . 1.6758(7) yes Si O3 . 1.6758(11) yes Si O1 . 1.6759(13) yes Si O1 8_455 1.6765(13) yes K O2 . 3.050(2) yes K O1 1_455 3.0513(14) yes K O2 1_455 3.364(2) yes K O1 8_455 3.3637(15) yes O4 H . 0.87(4) yes loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 Fe1 O3 5_656 2_656 95.65(4) yes O4 Fe1 O3 . 2_656 84.35(4) yes O3 Fe1 O3 2_656 5_656 94.56(5) yes O3 Fe1 O3 2_656 . 85.44(5) yes O4 Fe2 O4 5_656 1_655 82.73(5) yes O4 Fe2 O3 5_656 7_656 95.72(4) yes O4 Fe2 O3 1_655 7_656 178.14(4) ? O3 Fe2 O3 7_656 8 85.85(5) yes O3 Fe2 O3 8 2_756 85.70(4) yes O4 Fe2 O3 1_655 2_756 84.21(4) yes O4 Fe2 O3 1_655 . 95.16(4) yes O3 Fe2 O3 7_656 2_756 94.92(4) yes O3 Fe2 O3 2_756 . 179.16(5) ? O2 Si O3 . . 109.94(6) yes O2 Si O1 . . 109.05(8) yes O3 Si O1 . . 109.94(6) yes O2 Si O1 . 8_455 108.98(8) yes O3 Si O1 . 8_455 109.91(5) yes O1 Si O1 . 8_455 109.00(4) yes O2 K O2 . 5 180.00(6) ? O2 K O1 . 1_455 91.59(4) ? O2 K O1 5 1_455 88.41(4) ? O2 K O1 . 6_455 91.59(4) ? O2 K O1 5 6_455 88.41(4) ? O1 K O1 1_455 6_455 91.57(5) ? O2 K O1 . 2_655 88.41(4) ? O2 K O1 5 2_655 91.59(4) ? O1 K O1 1_455 2_655 88.43(5) ? O1 K O1 6_455 2_655 180.00(4) ? O2 K O1 . 5_655 88.41(4) ? O2 K O1 5 5_655 91.59(4) ? O1 K O1 1_455 5_655 180.00(5) ? O1 K O1 6_455 5_655 88.43(5) ? O1 K O1 2_655 5_655 91.57(5) ? O2 K O2 . 1_455 115.30(5) ? O2 K O2 5 1_455 64.70(5) ? O1 K O2 1_455 1_455 50.07(3) ? O1 K O2 6_455 1_455 50.07(3) ? O1 K O2 2_655 1_455 129.93(3) ? O1 K O2 5_655 1_455 129.93(3) ? O2 K O2 . 5_655 64.70(5) ? O2 K O2 5 5_655 115.30(5) ? O1 K O2 1_455 5_655 129.93(3) ? O1 K O2 6_455 5_655 129.93(3) ? O1 K O2 2_655 5_655 50.07(3) ? O1 K O2 5_655 5_655 50.07(3) ? O2 K O2 1_455 5_655 180.00(5) ? O2 K O1 . 8_455 50.06(2) ? O2 K O1 5 8_455 129.94(2) ? O1 K O1 1_455 8_455 50.067(17) ? O1 K O1 6_455 8_455 115.25(4) ? O1 K O1 2_655 8_455 64.75(4) ? O1 K O1 5_655 8_455 129.933(17) ? O2 K O1 1_455 8_455 96.40(3) ? O2 K O1 5_655 8_455 83.60(3) ? O2 K O1 . 4_545 129.94(2) ? O2 K O1 5 4_545 50.06(2) ? O1 K O1 1_455 4_545 129.933(17) ? O1 K O1 6_455 4_545 64.75(4) ? O1 K O1 2_655 4_545 115.25(4) ? O1 K O1 5_655 4_545 50.067(17) ? O2 K O1 1_455 4_545 83.60(3) ? O2 K O1 5_655 4_545 96.40(3) ? O1 K O1 8_455 4_545 180.00(4) ? O2 K O1 . 3_445 50.06(2) ? O2 K O1 5 3_445 129.94(2) ? O1 K O1 1_455 3_445 115.25(4) ? O1 K O1 6_455 3_445 50.067(17) ? O1 K O1 2_655 3_445 129.933(17) ? O1 K O1 5_655 3_445 64.75(4) ? O2 K O1 1_455 3_445 96.40(3) ? O2 K O1 5_655 3_445 83.60(3) ? O1 K O1 8_455 3_445 96.37(5) ? O1 K O1 4_545 3_445 83.63(5) ? O2 K O1 . 7 129.94(2) ? O2 K O1 5 7 50.06(2) ? O1 K O1 1_455 7 64.75(4) ? O1 K O1 6_455 7 129.933(17) ? O1 K O1 2_655 7 50.067(17) ? O1 K O1 5_655 7 115.25(4) ? O2 K O1 1_455 7 83.60(3) ? O2 K O1 5_655 7 96.40(3) ? O1 K O1 8_455 7 83.63(5) ? O1 K O1 4_545 7 96.37(5) ? O1 K O1 3_445 7 180.00(3) ? _journal_paper_doi 10.1107/S010827010400321X