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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
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data_I
_audit_creation_method     SHELXL97
_chemical_name_systematic
;
Goethite
;
_chemical_name_common     Goethite
_chemical_formula_moiety     'Fe H O2'
_chemical_formula_sum     'Fe H O2'
_chemical_formula_structural     'Fe O OH'
_chemical_formula_iupac     'Fe O (O H)'
_chemical_formula_weight     88.86
_chemical_melting_point     ?
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P b n m'
_symmetry_space_group_name_Hall     '-P 2c 2ab'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    'x+1/2, -y+1/2, -z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, z+1/2'
    '-x, -y, -z'
    '-x-1/2, y-1/2, z'
    'x-1/2, -y-1/2, z-1/2'
    'x, y, -z-1/2'
_cell_length_a     4.5979(2)
_cell_length_b     9.9510(5)
_cell_length_c     3.01780(10)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     138.076(10)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     1289
_cell_measurement_theta_min     2.5
_cell_measurement_theta_max     40.5
_cell_measurement_temperature     273(2)
_exptl_crystal_description     block
_exptl_crystal_colour     brown
_exptl_crystal_size_max     0.09
_exptl_crystal_size_mid     0.09
_exptl_crystal_size_min     0.08
_exptl_crystal_density_diffrn     4.275
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     172
_exptl_absorpt_coefficient_mu     10.301
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 2005)'
_exptl_absorpt_correction_T_min     0.410
_exptl_absorpt_correction_T_max     0.441
_exptl_special_details
;
;
_diffrn_ambient_temperature     273(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART APEX2 CCD area-detector'
_diffrn_measurement_method     'φ and ω'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     2197
_diffrn_reflns_av_R_equivalents     0.0172
_diffrn_reflns_av_sigmaI/netI     0.0145
_diffrn_reflns_theta_min     4.10
_diffrn_reflns_theta_max     40.48
_diffrn_reflns_theta_full     40.48
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -8
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_k_min     -17
_diffrn_reflns_limit_k_max     17
_diffrn_reflns_limit_l_min     -5
_diffrn_reflns_limit_l_max     5
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     483
_reflns_number_gt     458
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0197
_refine_ls_R_factor_gt     0.0186
_refine_ls_wR_factor_gt     0.0513
_refine_ls_wR_factor_ref     0.0518
_refine_ls_goodness_of_fit_ref     1.150
_refine_ls_restrained_S_all     1.150
_refine_ls_number_reflns     483
_refine_ls_number_parameters     23
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                     'w = 1/[σ²(Fo²)+(0.034P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.976
_refine_diff_density_min     -0.999
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_extinction_coef     0.087(9)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         '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'
_computing_data_collection     'SMART (Bruker, 2003)'
_computing_cell_refinement     'SAINT (Bruker, 2005)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'XtalDraw (Downs & Hall-Wallace, 2003)'
_computing_publication_material     'SHELXTL (Bruker, 1997)'
loop_
    _atom_site_type_symbol
    _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
    Fe Fe 0.04893(4) 0.853657(17) 0.2500 0.00588(8) Uani d S 1 . .
    O O1 0.7057(2) 0.19914(9) 0.2500 0.00717(16) Uani d S 1 . .
    O O2 0.1987(2) 0.05298(9) 0.2500 0.00740(17) Uani d S 1 . .
    H H 0.379(7) 0.082(3) 0.2500 0.017(6) Uiso d S 1 . .
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
    Fe 0.00664(11) 0.00537(11) 0.00565(11) 0.00004(4) 0.000 0.000
    O1 0.0071(3) 0.0073(3) 0.0072(4) 0.0020(3) 0.000 0.000
    O2 0.0069(3) 0.0064(3) 0.0089(4) -0.0004(3) 0.000 0.000
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
    Fe O1 6_665 1.9325(9) y
    Fe O1 5_666 1.9560(6) y
    Fe O1 5_665 1.9560(6) y
    Fe O2 1_565 2.0996(9) y
    Fe O2 5_565 2.1063(7) y
    Fe O2 5_566 2.1063(7) y
    O1 Fe 6_655 1.9325(9) ?
    O1 Fe 5_666 1.9560(6) ?
    O1 Fe 5_665 1.9560(6) ?
    O2 Fe 1_545 2.0996(9) ?
    O2 Fe 5_565 2.1063(7) ?
    O2 Fe 5_566 2.1063(7) ?
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
    O1 Fe O1 6_665 5_666 97.800(13) ?
    O1 Fe O1 6_665 5_665 97.800(13) ?
    O1 Fe O1 5_666 5_665 100.96(4) ?
    O1 Fe O2 6_665 1_565 161.87(4) ?
    O1 Fe O2 5_666 1_565 93.70(3) ?
    O1 Fe O2 5_665 1_565 93.70(3) ?
    O1 Fe O2 6_665 5_565 91.35(3) ?
    O1 Fe O2 5_666 5_565 169.41(4) ?
    O1 Fe O2 5_665 5_565 82.98(3) ?
    O2 Fe O2 1_565 5_565 76.15(3) ?
    O1 Fe O2 6_665 5_566 91.35(3) ?
    O1 Fe O2 5_666 5_566 82.98(3) ?
    O1 Fe O2 5_665 5_566 169.41(4) ?
    O2 Fe O2 1_565 5_566 76.15(3) ?
    O2 Fe O2 5_565 5_566 91.51(4) ?
    Fe O1 Fe 6_655 5_666 124.27(3) ?
    Fe O1 Fe 6_655 5_665 124.27(3) ?
    Fe O1 Fe 5_666 5_665 100.96(4) ?
    Fe O2 Fe 1_545 5_565 103.85(3) ?
    Fe O2 Fe 1_545 5_566 103.85(3) ?
    Fe O2 Fe 5_565 5_566 91.51(4) ?
data_global
_journal_date_recd_electronic     2006-10-11
_journal_date_accepted     2006-11-08
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2006
_journal_volume     62
_journal_issue     12
_journal_page_first     i250
_journal_page_last     i252
_journal_paper_category     EI
_journal_coeditor_code     WM2061
_publ_contact_author_name     'Hexiong Yang'
_publ_contact_author_address
;
Department of Geosciences
Gould-Simpson Building
University of Arizona
1040 East 4th Street
Tucson
AZ 85721-0077
USA
;
_publ_contact_author_email     hyang@u.arizona.edu
_publ_contact_author_fax     520-621-2672
_publ_contact_author_phone     520-621-9993
_publ_section_title
;
Goethite, α-FeO(OH), from single-crystal data
;
loop_
    _publ_author_name
    _publ_author_address
    'Yang, Hexiong'
;
University of Arizona
Department of Geosciences
1040 East 4th Street
Tucson
AZ 85721-0077
USA
;
    'Lu, Ren'
;
University of Arizona
Department of Geosciences
1040 East 4th Street
Tucson
AZ 85721-0077
USA
;
    'Downs, Robert T.'
;
University of Arizona
Department of Geosciences
1040 East 4th Street
Tucson
AZ 85721-0077
USA
;
    'Costin, Gelu'
;
University of Arizona
Department of Geosciences
1040 East 4th Street
Tucson
AZ 85721-0077
USA
;
