 
data_C133_S1_map_38_C23_rrp210512
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Fe2 S' 
_chemical_formula_weight          143.76

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Fe'  'Fe'   0.2886   0.5448
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.0826   0.0763
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n m a'
_space_group_name_Hall            '-P 2ac 2n'
 
_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'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    5.006(3)
_cell_length_b                    3.253(2)
_cell_length_c                    6.100(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      99.34(14)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used   117
_cell_measurement_theta_min     3.3870
_cell_measurement_theta_max     14.6490
 
_exptl_crystal_description        irregular
_exptl_crystal_colour             black
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     9.612          
_exptl_crystal_F_000              272
_exptl_transmission_factor_min    0.371
_exptl_transmission_factor_max    3.825
_exptl_crystal_size_max           0.0100
_exptl_crystal_size_mid           0.0100
_exptl_crystal_size_min           0.0100
_exptl_absorpt_coefficient_mu     2.55
_shelx_estimated_absorpt_T_min    0.88788
_shelx_estimated_absorpt_T_max    1.00000
_exptl_absorpt_correction_type            multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.29521
_diffrn_ambient_pressure          125000000
_diffrn_radiation_type            synchrotron
_diffrn_source                    synchrotron
_diffrn_measurement_device_type   '13IDD @ APS'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             214
_diffrn_reflns_av_unetI/netI      0.0178
_diffrn_reflns_av_R_equivalents   0.0186
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -3
_diffrn_reflns_limit_k_max        4
_diffrn_reflns_limit_l_min        -5
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          2.948
_diffrn_reflns_theta_max          14.954
_diffrn_reflns_theta_full         10.202
_diffrn_measured_fraction_theta_max   0.348
_diffrn_measured_fraction_theta_full  0.519
_diffrn_reflns_Laue_measured_fraction_max    0.348
_diffrn_reflns_Laue_measured_fraction_full   0.519
_diffrn_reflns_point_group_measured_fraction_max   0.348
_diffrn_reflns_point_group_measured_fraction_full  0.519
_reflns_number_total              110
_reflns_number_gt                 101
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.0701P)²+0.0449P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          110
_refine_ls_number_parameters      10
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0416
_refine_ls_R_factor_gt            0.0383
_refine_ls_wR_factor_ref          0.1020
_refine_ls_wR_factor_gt           0.1012
_refine_ls_goodness_of_fit_ref    1.175
_refine_ls_restrained_S_all       1.175
_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 0.0299(2) 0.7500 0.8247(3) 0.0056(4) Uiso 1 2 d S . P . .
Fe2 Fe 0.3524(2) 0.2500 0.9345(3) 0.0055(5) Uiso 1 2 d S . P . .
S1 S 1.2535(3) 0.2500 0.6180(5) 0.0054(5) Uiso 1 2 d S . 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 S1 2.092(3) 2_665 ?
Fe1 S1 2.1638(16) 6_457 ?
Fe1 S1 2.1638(16) 6_467 ?
Fe1 S1 2.343(2) 1_455 ?
Fe1 S1 2.343(2) 1_465 ?
Fe1 Fe2 2.3876(16) . ?
Fe1 Fe2 2.3877(16) 1_565 ?
Fe1 Fe2 2.413(2) 5_567 ?
Fe1 Fe2 2.436(2) 6_557 ?
Fe1 Fe2 2.436(2) 6_567 ?
Fe1 Fe2 2.452(3) 2_564 ?
Fe1 Fe1 2.6636(17) 6_657 ?
Fe2 S1 1.993(4) 1_455 ?
Fe2 S1 2.033(2) 6_557 ?
Fe2 S1 2.045(2) 2_665 ?
Fe2 S1 2.045(2) 2_655 ?
Fe2 Fe2 2.338(2) 5_667 ?
Fe2 Fe2 2.338(2) 5_657 ?
Fe2 Fe1 2.3876(16) 1_545 ?
Fe2 Fe1 2.413(2) 5_567 ?
Fe2 Fe1 2.436(2) 6_647 ?
Fe2 Fe1 2.436(2) 6_657 ?
Fe2 Fe1 2.452(3) 2_565 ?
S1 Fe2 1.993(4) 1_655 ?
S1 Fe2 2.033(2) 6_657 ?
S1 Fe2 2.045(2) 2_654 ?
S1 Fe2 2.045(2) 2_664 ?
S1 Fe1 2.092(3) 2_664 ?
S1 Fe1 2.1638(16) 6_757 ?
S1 Fe1 2.1638(16) 6_747 ?
S1 Fe1 2.343(2) 1_655 ?
S1 Fe1 2.343(2) 1_645 ?
 
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
S1 Fe1 S1 101.14(10) 2_665 6_457 ?
S1 Fe1 S1 101.14(10) 2_665 6_467 ?
S1 Fe1 S1 97.48(9) 6_457 6_467 ?
S1 Fe1 S1 102.28(7) 2_665 1_455 ?
S1 Fe1 S1 82.56(8) 6_457 1_455 ?
S1 Fe1 S1 156.12(10) 6_467 1_455 ?
S1 Fe1 S1 102.28(7) 2_665 1_465 ?
S1 Fe1 S1 156.12(10) 6_457 1_465 ?
S1 Fe1 S1 82.56(8) 6_467 1_465 ?
S1 Fe1 S1 87.94(11) 1_455 1_465 ?
S1 Fe1 Fe2 53.82(5) 2_665 . ?
S1 Fe1 Fe2 82.81(7) 6_457 . ?
S1 Fe1 Fe2 154.04(13) 6_467 . ?
S1 Fe1 Fe2 49.83(9) 1_455 . ?
S1 Fe1 Fe2 107.51(7) 1_465 . ?
S1 Fe1 Fe2 53.82(5) 2_665 1_565 ?
S1 Fe1 Fe2 154.04(13) 6_457 1_565 ?
S1 Fe1 Fe2 82.81(7) 6_467 1_565 ?
S1 Fe1 Fe2 107.51(7) 1_455 1_565 ?
S1 Fe1 Fe2 49.83(9) 1_465 1_565 ?
Fe2 Fe1 Fe2 85.88(8) . 1_565 ?
S1 Fe1 Fe2 83.70(11) 2_665 5_567 ?
S1 Fe1 Fe2 52.73(7) 6_457 5_567 ?
S1 Fe1 Fe2 52.73(7) 6_467 5_567 ?
S1 Fe1 Fe2 134.97(5) 1_455 5_567 ?
S1 Fe1 Fe2 134.97(5) 1_465 5_567 ?
Fe2 Fe1 Fe2 111.44(7) . 5_567 ?
Fe2 Fe1 Fe2 111.44(7) 1_565 5_567 ?
S1 Fe1 Fe2 138.08(5) 2_665 6_557 ?
S1 Fe1 Fe2 50.93(10) 6_457 6_557 ?
S1 Fe1 Fe2 111.94(10) 6_467 6_557 ?
S1 Fe1 Fe2 50.31(7) 1_455 6_557 ?
S1 Fe1 Fe2 106.77(11) 1_465 6_557 ?
Fe2 Fe1 Fe2 88.50(6) . 6_557 ?
Fe2 Fe1 Fe2 152.07(8) 1_565 6_557 ?
Fe2 Fe1 Fe2 96.08(6) 5_567 6_557 ?
S1 Fe1 Fe2 138.08(5) 2_665 6_567 ?
S1 Fe1 Fe2 111.94(10) 6_457 6_567 ?
S1 Fe1 Fe2 50.93(10) 6_467 6_567 ?
S1 Fe1 Fe2 106.77(11) 1_455 6_567 ?
S1 Fe1 Fe2 50.31(7) 1_465 6_567 ?
Fe2 Fe1 Fe2 152.07(8) . 6_567 ?
Fe2 Fe1 Fe2 88.50(6) 1_565 6_567 ?
Fe2 Fe1 Fe2 96.08(6) 5_567 6_567 ?
Fe2 Fe1 Fe2 83.77(10) 6_557 6_567 ?
S1 Fe1 Fe2 134.90(10) 2_665 2_564 ?
S1 Fe1 Fe2 108.08(10) 6_457 2_564 ?
S1 Fe1 Fe2 108.08(10) 6_467 2_564 ?
S1 Fe1 Fe2 50.42(7) 1_455 2_564 ?
S1 Fe1 Fe2 50.42(7) 1_465 2_564 ?
Fe2 Fe1 Fe2 96.31(6) . 2_564 ?
Fe2 Fe1 Fe2 96.31(6) 1_565 2_564 ?
Fe2 Fe1 Fe2 141.40(7) 5_567 2_564 ?
Fe2 Fe1 Fe2 57.15(7) 6_557 2_564 ?
Fe2 Fe1 Fe2 57.15(7) 6_567 2_564 ?
S1 Fe1 Fe1 78.80(9) 2_665 6_657 ?
S1 Fe1 Fe1 131.00(5) 6_457 6_657 ?
S1 Fe1 Fe1 131.00(5) 6_467 6_657 ?
S1 Fe1 Fe1 50.72(5) 1_455 6_657 ?
S1 Fe1 Fe1 50.72(5) 1_465 6_657 ?
Fe2 Fe1 Fe1 57.36(5) . 6_657 ?
Fe2 Fe1 Fe1 57.36(5) 1_565 6_657 ?
Fe2 Fe1 Fe1 162.50(11) 5_567 6_657 ?
Fe2 Fe1 Fe1 96.93(9) 6_557 6_657 ?
Fe2 Fe1 Fe1 96.93(9) 6_567 6_657 ?
Fe2 Fe1 Fe1 56.10(7) 2_564 6_657 ?
S1 Fe2 S1 95.32(10) 1_455 6_557 ?
S1 Fe2 S1 117.77(8) 1_455 2_665 ?
S1 Fe2 S1 110.03(7) 6_557 2_665 ?
S1 Fe2 S1 117.77(8) 1_455 2_655 ?
S1 Fe2 S1 110.03(7) 6_557 2_655 ?
S1 Fe2 S1 105.41(15) 2_665 2_655 ?
S1 Fe2 Fe2 119.21(8) 1_455 5_667 ?
S1 Fe2 Fe2 55.24(7) 6_557 5_667 ?
S1 Fe2 Fe2 54.79(6) 2_665 5_667 ?
S1 Fe2 Fe2 122.02(13) 2_655 5_667 ?
S1 Fe2 Fe2 119.21(8) 1_455 5_657 ?
S1 Fe2 Fe2 55.24(7) 6_557 5_657 ?
S1 Fe2 Fe2 122.02(13) 2_665 5_657 ?
S1 Fe2 Fe2 54.79(6) 2_655 5_657 ?
Fe2 Fe2 Fe2 88.16(9) 5_667 5_657 ?
S1 Fe2 Fe1 63.92(5) 1_455 . ?
S1 Fe2 Fe1 128.57(7) 6_557 . ?
S1 Fe2 Fe1 55.68(9) 2_665 . ?
S1 Fe2 Fe1 121.34(8) 2_655 . ?
Fe2 Fe2 Fe1 92.82(5) 5_667 . ?
Fe2 Fe2 Fe1 175.59(11) 5_657 . ?
S1 Fe2 Fe1 63.92(5) 1_455 1_545 ?
S1 Fe2 Fe1 128.58(7) 6_557 1_545 ?
S1 Fe2 Fe1 121.34(8) 2_665 1_545 ?
S1 Fe2 Fe1 55.68(9) 2_655 1_545 ?
Fe2 Fe2 Fe1 175.59(11) 5_667 1_545 ?
Fe2 Fe2 Fe1 92.82(5) 5_657 1_545 ?
Fe1 Fe2 Fe1 85.88(8) . 1_545 ?
S1 Fe2 Fe1 113.12(9) 1_455 5_567 ?
S1 Fe2 Fe1 151.56(13) 6_557 5_567 ?
S1 Fe2 Fe1 57.37(7) 2_665 5_567 ?
S1 Fe2 Fe1 57.37(7) 2_655 5_567 ?
Fe2 Fe2 Fe1 107.05(10) 5_667 5_567 ?
Fe2 Fe2 Fe1 107.05(10) 5_657 5_567 ?
Fe1 Fe2 Fe1 68.56(7) . 5_567 ?
Fe1 Fe2 Fe1 68.56(7) 1_545 5_567 ?
S1 Fe2 Fe1 57.44(7) 1_455 6_647 ?
S1 Fe2 Fe1 62.46(7) 6_557 6_647 ?
S1 Fe2 Fe1 168.85(8) 2_665 6_647 ?
S1 Fe2 Fe1 85.35(9) 2_655 6_647 ?
Fe2 Fe2 Fe1 117.12(9) 5_667 6_647 ?
Fe2 Fe2 Fe1 61.77(8) 5_657 6_647 ?
Fe1 Fe2 Fe1 121.29(8) . 6_647 ?
Fe1 Fe2 Fe1 67.03(5) 1_545 6_647 ?
Fe1 Fe2 Fe1 133.19(4) 5_567 6_647 ?
S1 Fe2 Fe1 57.44(7) 1_455 6_657 ?
S1 Fe2 Fe1 62.46(7) 6_557 6_657 ?
S1 Fe2 Fe1 85.35(9) 2_665 6_657 ?
S1 Fe2 Fe1 168.85(8) 2_655 6_657 ?
Fe2 Fe2 Fe1 61.77(8) 5_667 6_657 ?
Fe2 Fe2 Fe1 117.12(9) 5_657 6_657 ?
Fe1 Fe2 Fe1 67.03(5) . 6_657 ?
Fe1 Fe2 Fe1 121.29(8) 1_545 6_657 ?
Fe1 Fe2 Fe1 133.19(4) 5_567 6_657 ?
Fe1 Fe2 Fe1 83.77(10) 6_647 6_657 ?
S1 Fe2 Fe1 179.51(7) 1_455 2_565 ?
S1 Fe2 Fe1 85.17(10) 6_557 2_565 ?
S1 Fe2 Fe1 62.02(9) 2_665 2_565 ?
S1 Fe2 Fe1 62.02(9) 2_655 2_565 ?
Fe2 Fe2 Fe1 61.08(7) 5_667 2_565 ?
Fe2 Fe2 Fe1 61.08(7) 5_657 2_565 ?
Fe1 Fe2 Fe1 115.77(6) . 2_565 ?
Fe1 Fe2 Fe1 115.77(6) 1_545 2_565 ?
Fe1 Fe2 Fe1 66.39(7) 5_567 2_565 ?
Fe1 Fe2 Fe1 122.85(7) 6_647 2_565 ?
Fe1 Fe2 Fe1 122.85(7) 6_657 2_565 ?
Fe2 S1 Fe2 113.45(13) 1_655 6_657 ?
Fe2 S1 Fe2 126.50(8) 1_655 2_654 ?
Fe2 S1 Fe2 69.97(7) 6_657 2_654 ?
Fe2 S1 Fe2 126.50(8) 1_655 2_664 ?
Fe2 S1 Fe2 69.97(7) 6_657 2_664 ?
Fe2 S1 Fe2 105.41(15) 2_654 2_664 ?
Fe2 S1 Fe1 134.41(11) 1_655 2_664 ?
Fe2 S1 Fe1 112.14(15) 6_657 2_664 ?
Fe2 S1 Fe1 70.50(10) 2_654 2_664 ?
Fe2 S1 Fe1 70.50(10) 2_664 2_664 ?
Fe2 S1 Fe1 71.62(9) 1_655 6_757 ?
Fe2 S1 Fe1 131.06(4) 6_657 6_757 ?
Fe2 S1 Fe1 148.47(15) 2_654 6_757 ?
Fe2 S1 Fe1 69.90(7) 2_664 6_757 ?
Fe1 S1 Fe1 78.86(10) 2_664 6_757 ?
Fe2 S1 Fe1 71.62(9) 1_655 6_747 ?
Fe2 S1 Fe1 131.06(4) 6_657 6_747 ?
Fe2 S1 Fe1 69.90(7) 2_654 6_747 ?
Fe2 S1 Fe1 148.47(15) 2_664 6_747 ?
Fe1 S1 Fe1 78.86(10) 2_664 6_747 ?
Fe1 S1 Fe1 97.48(9) 6_757 6_747 ?
Fe2 S1 Fe1 66.26(9) 1_655 1_655 ?
Fe2 S1 Fe1 67.23(7) 6_657 1_655 ?
Fe2 S1 Fe1 136.30(9) 2_654 1_655 ?
Fe2 S1 Fe1 67.56(8) 2_664 1_655 ?
Fe1 S1 Fe1 135.06(7) 2_664 1_655 ?
Fe1 S1 Fe1 72.34(6) 6_757 1_655 ?
Fe1 S1 Fe1 137.77(15) 6_747 1_655 ?
Fe2 S1 Fe1 66.26(9) 1_655 1_645 ?
Fe2 S1 Fe1 67.23(7) 6_657 1_645 ?
Fe2 S1 Fe1 67.56(8) 2_654 1_645 ?
Fe2 S1 Fe1 136.30(9) 2_664 1_645 ?
Fe1 S1 Fe1 135.06(7) 2_664 1_645 ?
Fe1 S1 Fe1 137.77(15) 6_757 1_645 ?
Fe1 S1 Fe1 72.34(6) 6_747 1_645 ?
Fe1 S1 Fe1 87.94(11) 1_655 1_645 ?
 
 
_refine_diff_density_max    1.367
_refine_diff_density_min   -1.658
_refine_diff_density_rms    0.426


# start Validation Reply Form
_vrf_ATOM007_C133_S1_map_38_C23_rrp210512
;
PROBLEM: _atom_site_aniso_label is missing
            Unique label identifying the atom site. 
RESPONSE: The structure was refined isotropically
;
_vrf_PLAT029_C133_S1_map_38_C23_rrp210512
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.558 Why?  
RESPONSE: The limited x-ray opening of the DAC and modest strain of the crystal
 are at the origin of the low resolution.
;
_vrf_PLAT973_C133_S1_map_38_C23_rrp210512
;
PROBLEM: Check Calcd Positive Resid. Density on       Fe2        3.21 eA-3 
RESPONSE: Microdifffraction data collected in the DAC are affected by well-known
 issues  measured structure factors, while these are not systematic, they
 typically result in less-than ideal refinements. 
;
_vrf_PLAT927_C133_C133_S1_map_38_C23_rrp210512
;
PROBLEM: Reported and Calculated   wR2 Differ by .........    -0.0098 Check 
RESPONSE: Data quality at high pressures affected the quality of the refinement.
;
_vrf_PLAT926_C133_S1_map_38_C23_rrp210512
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0089 Check 
RESPONSE: Data quality at high pressures affected the quality of the refinement.
;
_vrf_PLAT911_C133_S1_map_38_C23_rrp210512
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         45 Report
RESPONSE: Completeness of data is limited by shading of detector by diamond
 anvil cell.
;
# end Validation Reply Form
