 
data_shelx
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'parahibbingite'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H3 Cl Fe2 O3' 
_chemical_formula_weight          198.17

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            166
_space_group_name_H-M_alt         'R -3 m :H'
_space_group_name_Hall            '-R 3 2"'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'y+2/3, x+1/3, -z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '-x+2/3, -x+y+1/3, -z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 'y+1/3, x+2/3, -z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-y+2/3, -x+1/3, z+1/3'
 '-x+y+2/3, y+1/3, z+1/3'
 'x+2/3, x-y+1/3, z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 '-y+1/3, -x+2/3, z+2/3'
 '-x+y+1/3, y+2/3, z+2/3'
 'x+1/3, x-y+2/3, z+2/3'
 
_cell_length_a                    6.9362(4)
_cell_length_b                    6.9362(4)
_cell_length_c                    14.6730(11)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      611.35(9)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     425 
_cell_measurement_theta_min       10.2 
_cell_measurement_theta_max       27.8 
 
_exptl_crystal_description        block
_exptl_crystal_colour             orange
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     3.230          
_exptl_crystal_F_000              576
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.07
_exptl_absorpt_coefficient_mu     7.613
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    'gaussian'
_exptl_absorpt_correction_T_min   0.490 
_exptl_absorpt_correction_T_max   0.599
_exptl_absorpt_process_details    
'(ABSPACK; Oxford Diffraction, 2006)' 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                        
_diffrn_measurement_device_type   'D8 Advance diffractometer'
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             1616
_diffrn_reflns_av_unetI/netI      0.0377
_diffrn_reflns_av_R_equivalents   0.0395
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          4.167
_diffrn_reflns_theta_max          36.832
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.973
_diffrn_measured_fraction_theta_full  0.994
_diffrn_reflns_Laue_measured_fraction_max    0.973
_diffrn_reflns_Laue_measured_fraction_full   0.994
_diffrn_reflns_point_group_measured_fraction_max   0.973
_diffrn_reflns_point_group_measured_fraction_full  0.994
_reflns_number_total              402
_reflns_number_gt                 320
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0340P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refxyz
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          402
_refine_ls_number_parameters      18
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0495
_refine_ls_R_factor_gt            0.0331
_refine_ls_wR_factor_ref          0.0770
_refine_ls_wR_factor_gt           0.0703
_refine_ls_goodness_of_fit_ref    1.098
_refine_ls_restrained_S_all       1.101
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.5000 0.0135(2) Uani 1 12 d S T P . .
Fe2 Fe 0.5000 0.0000 0.0000 0.01451(17) Uani 1 4 d S T P . .
O O 0.20145(19) 0.79855(19) 0.06872(15) 0.0168(4) Uani 1 2 d DS T P . .
Cl Cl 0.0000 0.0000 0.21651(8) 0.0172(2) Uani 1 6 d S T P . .
H H 0.1335(19) 0.8665(19) 0.088(2) 0.025 Uiso 1 2 d DS U P . .
 
 
_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
Fe1 O 2.139(2) 32_445 ?
Fe1 O 2.139(2) 8 ?
Fe1 O 2.139(2) 33_545 ?
Fe1 O 2.139(2) 9_455 ?
Fe1 O 2.139(2) 31 ?
Fe1 O 2.139(2) 7_445 ?
Fe2 O 2.0890(12) 19_665 ?
Fe2 O 2.0890(12) 1_545 ?
Fe2 O 2.0890(12) 21_655 ?
Fe2 O 2.0890(12) 3 ?
Fe2 Cl 2.6358(8) 25 ?
Fe2 Cl 2.6358(8) 13_544 ?
O H 0.864(19) . ?
O Fe2 2.0890(12) 2 ?
O Fe2 2.0890(12) 1_565 ?
O Fe1 2.139(2) 13_554 ?
Cl Fe2 2.6358(8) 9 ?
Cl Fe2 2.6358(8) 7_455 ?
Cl Fe2 2.6358(8) 8_445 ?
 
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 Fe1 O 180.0 32_445 8 ?
O Fe1 O 79.81(9) 32_445 33_545 ?
O Fe1 O 100.19(9) 8 33_545 ?
O Fe1 O 100.19(9) 32_445 9_455 ?
O Fe1 O 79.81(9) 8 9_455 ?
O Fe1 O 180.0 33_545 9_455 ?
O Fe1 O 79.80(9) 32_445 31 ?
O Fe1 O 100.20(9) 8 31 ?
O Fe1 O 79.80(9) 33_545 31 ?
O Fe1 O 100.20(9) 9_455 31 ?
O Fe1 O 100.20(9) 32_445 7_445 ?
O Fe1 O 79.80(9) 8 7_445 ?
O Fe1 O 100.20(9) 33_545 7_445 ?
O Fe1 O 79.80(9) 9_455 7_445 ?
O Fe1 O 180.00(9) 31 7_445 ?
O Fe2 O 180.00(13) 19_665 1_545 ?
O Fe2 O 82.12(12) 19_665 21_655 ?
O Fe2 O 97.88(13) 1_545 21_655 ?
O Fe2 O 97.88(13) 19_665 3 ?
O Fe2 O 82.12(13) 1_545 3 ?
O Fe2 O 180.00(12) 21_655 3 ?
O Fe2 Cl 82.75(5) 19_665 25 ?
O Fe2 Cl 97.25(5) 1_545 25 ?
O Fe2 Cl 82.75(5) 21_655 25 ?
O Fe2 Cl 97.25(5) 3 25 ?
O Fe2 Cl 97.25(5) 19_665 13_544 ?
O Fe2 Cl 82.75(5) 1_545 13_544 ?
O Fe2 Cl 97.25(5) 21_655 13_544 ?
O Fe2 Cl 82.75(5) 3 13_544 ?
Cl Fe2 Cl 180.00(4) 25 13_544 ?
H O Fe2 115.0(10) . 2 ?
H O Fe2 115.0(10) . 1_565 ?
Fe2 O Fe2 112.22(10) 2 1_565 ?
H O Fe1 119(3) . 13_554 ?
Fe2 O Fe1 96.74(7) 2 13_554 ?
Fe2 O Fe1 96.74(7) 1_565 13_554 ?
Fe2 Cl Fe2 82.28(3) 9 7_455 ?
Fe2 Cl Fe2 82.28(3) 9 8_445 ?
Fe2 Cl Fe2 82.28(3) 7_455 8_445 ?
 
_refine_diff_density_max    1.346
_refine_diff_density_min   -1.107
_refine_diff_density_rms    0.189

_shelxl_version_number 2013-4



