#============================================================================== 

data_New_Global_Publ_Block

# start Validation Reply Form
_vrf_ATOM007_shelxl
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: no anisotropic refinements of adp's carried out due to small number of reflections
;
_vrf_REFLT03_shelxl
;
PROBLEM: Reflection count < 85% complete (theta max?)
RESPONSE: completeness low lower than expected due to limited opening angle of the diamond anvil cell
;
_vrf_PLAT022_shelxl
;
PROBLEM: Ratio Unique / Expected Reflections too Low ....       0.60      
RESPONSE: number of observed reflections lower than expected due to limited opening angle of the diamond anvil cell
;
_vrf_PLAT029_shelxl
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......       0.59      
RESPONSE: number of observed reflections lower than expected due to limited opening angle of the diamond anvil cell
;
_vrf_ABSTY01_shelxl
;
PROBLEM: The absorption correction should be one of the following
RESPONSE: no absorption correction necessary as it would not improve the data due a beamsize of approximately 5 x 5 µm, the crystal being a platelet of about 10-15 µm thick and the Diamond Anvil Cell environment. 
;
# end Validation Reply Form

#Added by publCIF (Mon Dec 27 11:55:05 2010)


#==============================================================================
 
data_shelxl 
 
_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'   0.0018   0.0018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Fe'  'Fe'   0.2000   0.3092 
 '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                    4.9702(3) 
_cell_length_b                    4.9702(3) 
_cell_length_c                    13.5180(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      289.20(4) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     293(2) 
_cell_measurement_pressure        95(1)
_cell_measurement_reflns_used     41
_cell_measurement_theta_min       3 
_cell_measurement_theta_max       15 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.040
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           0.015
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.502 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              456 
_exptl_absorpt_coefficient_mu     3.029 
_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_ambient_pressure          95(1)
_diffrn_radiation_wavelength      0.41530 
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'synchrotron' 
_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             87 
_diffrn_reflns_av_R_equivalents   0.0109 
_diffrn_reflns_av_sigmaI/netI     0.0088 
_diffrn_reflns_limit_h_min        -4 
_diffrn_reflns_limit_h_max        5 
_diffrn_reflns_limit_k_min        -4 
_diffrn_reflns_limit_k_max        4 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.28 
_diffrn_reflns_theta_max          15.09 
_reflns_number_total              41 
_reflns_number_gt                 40 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0396P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_number_reflns          41 
_refine_ls_number_parameters      6 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0236 
_refine_ls_R_factor_gt            0.0228 
_refine_ls_wR_factor_ref          0.0583 
_refine_ls_wR_factor_gt           0.0581 
_refine_ls_goodness_of_fit_ref    1.264 
_refine_ls_restrained_S_all       1.264 
_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 0.35548(10) 0.0103(8) Uiso 1 3 d S . . 
O O 0.3064(6) 0.0000 0.2500 0.0120(13) Uiso 1 2 d S . . 
 
_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 1.9153(14) 34_445 ? 
Fe O 1.9153(14) 32 ? 
Fe O 1.9154(14) 31_545 ? 
Fe O 2.086(2) . ? 
Fe O 2.086(2) 4 ? 
Fe O 2.086(2) 2 ? 
Fe Fe 2.852(3) 3 ? 
Fe Fe 2.9313(6) 31_445 ? 
Fe Fe 2.9313(6) 31 ? 
Fe Fe 2.9314(6) 31_545 ? 
O Fe 1.9153(14) 27 ? 
O Fe 1.9154(14) 31_545 ? 
O Fe 2.086(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 102.73(5) 34_445 32 ? 
O Fe O 102.72(5) 34_445 31_545 ? 
O Fe O 102.72(5) 32 31_545 ? 
O Fe O 162.19(11) 34_445 . ? 
O Fe O 90.28(6) 32 . ? 
O Fe O 85.90(3) 31_545 . ? 
O Fe O 85.90(3) 34_445 4 ? 
O Fe O 162.19(11) 32 4 ? 
O Fe O 90.28(6) 31_545 4 ? 
O Fe O 78.42(10) . 4 ? 
O Fe O 90.28(6) 34_445 2 ? 
O Fe O 85.90(3) 32 2 ? 
O Fe O 162.19(11) 31_545 2 ? 
O Fe O 78.42(10) . 2 ? 
O Fe O 78.42(10) 4 2 ? 
O Fe Fe 115.58(4) 34_445 3 ? 
O Fe Fe 115.58(4) 32 3 ? 
O Fe Fe 115.58(4) 31_545 3 ? 
O Fe Fe 46.88(6) . 3 ? 
O Fe Fe 46.89(6) 4 3 ? 
O Fe Fe 46.89(6) 2 3 ? 
O Fe Fe 45.22(6) 34_445 31_445 ? 
O Fe Fe 145.24(6) 32 31_445 ? 
O Fe Fe 98.48(7) 31_545 31_445 ? 
O Fe Fe 118.64(9) . 31_445 ? 
O Fe Fe 40.67(4) 4 31_445 ? 
O Fe Fe 81.98(4) 2 31_445 ? 
Fe Fe Fe 78.21(5) 3 31_445 ? 
O Fe Fe 98.48(7) 34_445 31 ? 
O Fe Fe 45.22(6) 32 31 ? 
O Fe Fe 145.24(7) 31_545 31 ? 
O Fe Fe 81.97(4) . 31 ? 
O Fe Fe 118.64(9) 4 31 ? 
O Fe Fe 40.67(4) 2 31 ? 
Fe Fe Fe 78.21(5) 3 31 ? 
Fe Fe Fe 115.94(3) 31_445 31 ? 
O Fe Fe 145.24(6) 34_445 31_545 ? 
O Fe Fe 98.48(7) 32 31_545 ? 
O Fe Fe 45.22(6) 31_545 31_545 ? 
O Fe Fe 40.67(4) . 31_545 ? 
O Fe Fe 81.98(4) 4 31_545 ? 
O Fe Fe 118.64(9) 2 31_545 ? 
Fe Fe Fe 78.21(5) 3 31_545 ? 
Fe Fe Fe 115.94(3) 31_445 31_545 ? 
Fe Fe Fe 115.94(4) 31 31_545 ? 
Fe O Fe 119.69(15) 27 31_545 ? 
Fe O Fe 131.44(4) 27 . ? 
Fe O Fe 94.11(3) 31_545 . ? 
Fe O Fe 94.10(3) 27 3 ? 
Fe O Fe 131.44(4) 31_545 3 ? 
Fe O Fe 86.23(13) . 3 ? 
 
_diffrn_measured_fraction_theta_max    0.594 
_diffrn_reflns_theta_full              15.09 
_diffrn_measured_fraction_theta_full   0.594 
_refine_diff_density_max    0.570 
_refine_diff_density_min   -0.805 
_refine_diff_density_rms    0.156 
