#------------------------------------------------------------------------------
#$Date: 2015-01-27 20:58:39 +0100 (mar 27 de ene de 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000330.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_4000330
loop_
_publ_author_name
'Gaillot, Anne-Claire'
'Flot, David'
'Drits, Victor A.'
'Burghammer, Manfred'
'Manceau, Alain'
'Lanson, Bruno'
_publ_section_title
;
 Structure of synthetic K-rich birnessite obtained by high-temperature
decomposition of KMnO4.
I. Two-layer polytype from 800 C experiments.
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm021733g
_journal_year                    2003
_chemical_formula_moiety         'K1 Mn2 O5'
_chemical_formula_sum            'K Mn2 O5.44'
_chemical_formula_weight         236.02
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   2.840(1)
_cell_length_b                   2.840(1)
_cell_length_c                   14.030(6)
_cell_measurement_reflns_used    1523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      8.52
_cell_volume                     98.00(6)
_diffrn_detector_area_resol_mean 15.52
_diffrn_detector_type            marCCD
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'ESRF/EMBL microdiffractometer'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'ESRF-ID13 beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.729
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6727
_diffrn_reflns_theta_full        41.4
_diffrn_reflns_theta_max         41.4
_diffrn_reflns_theta_min         8.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.415
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             113
_exptl_crystal_size_max          0.003
_exptl_crystal_size_mid          0.003
_exptl_crystal_size_min          0.0005
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.393
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0344P)²+0.1787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                137
_reflns_number_total             153
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4000330
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'
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)
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'
