data_4000330 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _publ_section_title ; Structure of synthetic K-rich birnessite obtained by high-temperature decomposition of KMnO4. I. Two-layer polytype from 800 C experiments. ; loop_ _publ_author_name 'Gaillot, Anne-Claire' 'Flot, David' 'Drits, Victor A.' 'Burghammer, Manfred' 'Manceau, Alain' 'Lanson, Bruno' _chemical_formula_moiety 'K1 Mn2 O5' _chemical_formula_sum 'K Mn2 O5.44' _chemical_formula_weight 236.02 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 2.840(1) _cell_length_b 2.840(1) _cell_length_c 14.030(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 98.00(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1523 _cell_measurement_theta_min 8.52 _cell_measurement_theta_max 27.8 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.003 _exptl_crystal_size_mid 0.003 _exptl_crystal_size_min 0.0005 _exptl_crystal_density_diffrn 3.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 113 _exptl_absorpt_coefficient_mu 7.415 _exptl_absorpt_correction_type none _diffrn_radiation_type synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_source 'ESRF-ID13 beamline' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'ESRF/EMBL microdiffractometer' _diffrn_measurement_method oscillation _diffrn_detector_type 'marCCD' _diffrn_detector_area_resol_mean '15.52' _diffrn_standards_number 0 _diffrn_radiation_wavelength 0.729 _diffrn_reflns_number 6727 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 8.52 _diffrn_reflns_theta_max 41.4 _diffrn_reflns_theta_full 41.4 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _reflns_number_total 153 _reflns_number_gt 137 _reflns_threshold_expression >2sigma(I) 'WinGX publication routines (Farrugia, 1999)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.1787P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 153 _refine_ls_number_parameters 14 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0696 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0 _refine_diff_density_max 0.971 _refine_diff_density_min -0.393 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Mn1 Mn 0 0 0 0.01237(18) Uani 0.89 d SP . . O1 O 0.6667 0.3333 0.07040(15) 0.0173(4) Uiso 1 d S . . K1 K 0.227(6) 0.773(6) 0.25 0.094(9) Uani 0.08 d SP . . Mn2 Mn 0 0 0.1506(12) 0.025(3) Uiso 0.04 d SP . . O2 O 0.3333 0.6667 0.25 0.08(2) Uiso 0.23 d SP . . O3 O 0.226(13) 0.113(7) 0.25 0.047(7) Uiso 0.12 d SP . . 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 0.0115(2) 0.0115(2) 0.0141(3) 0 0 0.00577(10) K1 0.158(17) 0.158(17) 0.0082(18) 0 0 0.110(18)