data_fe2o3_frd # start Validation Reply Form _vrf_PUBL004_GLOBAL ; PROBLEM: The contact author's name and address are missing, RESPONSE: ... ; _vrf_PUBL005_GLOBAL ; PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and RESPONSE: ... ; _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: ... ; _vrf_PUBL008_GLOBAL ; PROBLEM: _publ_section_title is missing. Title of paper. RESPONSE: ... ; _vrf_PUBL009_GLOBAL ; PROBLEM: _publ_author_name is missing. List of author(s) name(s). RESPONSE: ... ; _vrf_PUBL010_GLOBAL ; PROBLEM: _publ_author_address is missing. Author(s) address(es). RESPONSE: ... ; _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: ... ; _vrf_SYMM001_fe2o3_frd ; PROBLEM: _symmetry_cell_setting is missing RESPONSE: ... ; _vrf_EXPT005_fe2o3_frd ; PROBLEM: _exptl_crystal_description is missing RESPONSE: ... ; _vrf_DIFF005_fe2o3_frd ; PROBLEM: _diffrn_measurement_method is missing RESPONSE: ... ; _vrf_DIFF019_fe2o3_frd ; PROBLEM: _diffrn_standards_number is missing RESPONSE: ... ; _vrf_DIFF020_fe2o3_frd ; PROBLEM: _diffrn_standards_interval_count and RESPONSE: ... ; _vrf_DIFF022_fe2o3_frd ; PROBLEM: _diffrn_standards_decay_% is missing RESPONSE: ... ; # end Validation Reply Form #Added by publCIF (Mon Dec 27 15:55:58 2010) # start Validation Reply Form _vrf_ABSTY01_fe2o3_frd ; PROBLEM: The absorption correction should be one of the following RESPONSE: No absorption correction applied, the sample had thickness of approximately 15 µm and was located in a diamond anvil cell. Synchrotron measurements were perofrmed with a beamsize of roughly 5 x 5 µm. Total thickness of diamonds amounted to roughley 4-4.5 mm. It was assumed that an absorption correction would certainly not improve the data. The in house measurement was conducted on the same sample and DAC and thus was also not corrected. ; _vrf_PLAT940_fe2o3_frd ; PROBLEM: F**2 Refinement with I .GT. n * Sigma(I) only .. ? RESPONSE: The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. ; _vrf_PLAT052_fe2o3_frd ; PROBLEM: (Proper) Absorption Correction Method Missing .. ? RESPONSE: No absorption correction applied, the sample had thickness of approximately 15 µm and was located in a diamond anvil cell. Synchrotron measurements were perofrmed with a beamsize of roughly 5 x 5 µm. Total thickness of diamonds amounted to roughley 4-4.5 mm. It was assumed that an absorption correction would certainly not improve the data. The in house measurement was conducted on the same sample and DAC and thus was also not corrected. ; # end Validation Reply Form #Added by publCIF (Mon Dec 27 15:36:10 2010) _audit_update_record ; 2010-12-27 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common Hematite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Fe2 O3' _chemical_formula_weight 159.70 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'R -3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 5.0354(17) _cell_length_b 5.0354(17) _cell_length_c 13.748(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 301.88(18) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 82 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 14.067 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71065 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type DAC _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 387 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.53 _diffrn_reflns_theta_max 27.85 _reflns_number_total 82 _reflns_number_gt 82 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0688P)^2^+0.1327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_number_reflns 82 _refine_ls_number_parameters 6 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.0000 0.0000 0.35523(7) 0.0106(11) Uani 1 3 d S . . O O 0.3059(5) 0.0000 0.2500 0.0132(13) Uani 1 2 d S . . 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 Fe 0.0088(12) 0.0088(12) 0.0141(16) 0.000 0.000 0.0044(6) O 0.0111(14) 0.0116(14) 0.0171(18) 0.0015(5) 0.0007(3) 0.0058(7) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O 1.9447(16) 34_445 ? Fe O 1.9447(16) 32 ? Fe O 1.9447(16) 31_545 ? Fe O 2.113(2) 4 ? Fe O 2.113(2) 2 ? Fe O 2.113(2) . ? Fe Fe 2.893(2) 3 ? Fe Fe 2.9689(10) 31_445 ? Fe Fe 2.9689(10) 31 ? Fe Fe 2.9689(10) 31_545 ? O Fe 1.9447(16) 27 ? O Fe 1.9447(16) 31_545 ? O Fe 2.113(2) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Fe O 102.54(4) 34_445 32 ? O Fe O 102.54(4) 34_445 31_545 ? O Fe O 102.54(4) 32 31_545 ? O Fe O 86.04(3) 34_445 4 ? O Fe O 162.24(9) 32 4 ? O Fe O 90.50(6) 31_545 4 ? O Fe O 90.50(6) 34_445 2 ? O Fe O 86.04(3) 32 2 ? O Fe O 162.24(9) 31_545 2 ? O Fe O 78.28(8) 4 2 ? O Fe O 162.24(9) 34_445 . ? O Fe O 90.50(6) 32 . ? O Fe O 86.04(3) 31_545 . ? O Fe O 78.28(8) 4 . ? O Fe O 78.28(8) 2 . ? O Fe Fe 115.74(3) 34_445 3 ? O Fe Fe 115.74(3) 32 3 ? O Fe Fe 115.74(3) 31_545 3 ? O Fe Fe 46.79(5) 4 3 ? O Fe Fe 46.79(5) 2 3 ? O Fe Fe 46.79(5) . 3 ? O Fe Fe 45.24(6) 34_445 31_445 ? O Fe Fe 145.09(6) 32 31_445 ? O Fe Fe 98.53(6) 31_545 31_445 ? O Fe Fe 40.80(4) 4 31_445 ? O Fe Fe 82.02(3) 2 31_445 ? O Fe Fe 118.64(6) . 31_445 ? Fe Fe Fe 78.30(4) 3 31_445 ? O Fe Fe 98.54(6) 34_445 31 ? O Fe Fe 45.24(6) 32 31 ? O Fe Fe 145.08(6) 31_545 31 ? O Fe Fe 118.64(6) 4 31 ? O Fe Fe 40.80(4) 2 31 ? O Fe Fe 82.02(3) . 31 ? Fe Fe Fe 78.30(4) 3 31 ? Fe Fe Fe 116.00(2) 31_445 31 ? O Fe Fe 145.08(6) 34_445 31_545 ? O Fe Fe 98.53(6) 32 31_545 ? O Fe Fe 45.24(6) 31_545 31_545 ? O Fe Fe 82.02(3) 4 31_545 ? O Fe Fe 118.64(6) 2 31_545 ? O Fe Fe 40.80(4) . 31_545 ? Fe Fe Fe 78.30(4) 3 31_545 ? Fe Fe Fe 116.00(2) 31_445 31_545 ? Fe Fe Fe 116.00(2) 31 31_545 ? Fe O Fe 119.64(14) 27 31_545 ? Fe O Fe 93.96(3) 27 3 ? Fe O Fe 131.59(4) 31_545 3 ? Fe O Fe 131.58(4) 27 . ? Fe O Fe 93.96(3) 31_545 . ? Fe O Fe 86.42(11) 3 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.622 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.319