data_cmosk3_pos1_oli
_audit_creation_date               2023-08-04
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'Fe0.143 Mg1.857 O4 Si'
_chemical_formula_sum              'Fe0.16 Mg1.84 O-4 Si'
_chemical_formula_weight           145.82
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Fe' 'Fe+2' 0.2000 0.3040
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mg' 'Mg+2' 0.0150 0.0120
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O-2' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si' 'Si+4' 0.0270 0.0230
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             62
_space_group_name_H-M_alt          'P b n m'
_space_group_name_Hall             '-P 2c 2ab'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 'x, y, -z-1/2'
 '-x-1/2, y-1/2, z'

_cell_length_a                     4.7568(4)
_cell_length_b                     10.183(2)
_cell_length_c                     5.9885(4)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       290.06(7)
_cell_formula_units_Z              4
_audit_creation_method         'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection     'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_cell_refinement     'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction      'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_cell_measurement_reflns_used   132
_cell_measurement_theta_min     2.7470
_cell_measurement_theta_max     16.1200
_cell_measurement_temperature   293(2)
_cell_oxdiff_length_a                  4.7570(9) 
_cell_oxdiff_length_b                  5.9877(6) 
_cell_oxdiff_length_c                  10.185(2) 
_cell_oxdiff_angle_alpha               89.981(13) 
_cell_oxdiff_angle_beta                89.998(16) 
_cell_oxdiff_angle_gamma               90.016(11) 
_cell_oxdiff_volume                    290.12(9) 
_cell_oxdiff_measurement_reflns_used   132
_exptl_absorpt_correction_T_min                   0.58812
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min           0.760
_oxdiff_exptl_absorpt_empirical_full_max           1.259
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_source synchrotron
_diffrn_radiation_probe x-ray
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.41330
_diffrn_radiation_monochromator synchrotron
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type 'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector 'CCD plate'
_diffrn_reflns_number 362
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_theta_min 2.4900
_diffrn_reflns_theta_max 16.8653
_diffrn_measured_fraction_theta_max 0.3563
_diffrn_reflns_theta_full 14.9700
_diffrn_measured_fraction_theta_full 0.4621
_diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0432139000
_diffrn_orient_matrix_UB_12      -0.0165370000
_diffrn_orient_matrix_UB_13      -0.0338308000
_diffrn_orient_matrix_UB_21       0.0715706000
_diffrn_orient_matrix_UB_22      -0.0297884000
_diffrn_orient_matrix_UB_23      -0.0149032000
_diffrn_orient_matrix_UB_31      -0.0236378000
_diffrn_orient_matrix_UB_32      -0.0600296000
_diffrn_orient_matrix_UB_33       0.0167306000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      0.00  80.00   0.50    1.00    --    0.00   0.00   0.00  160
;
_shelx_estimated_absorpt_T_max     0.975
_shelx_estimated_absorpt_T_min     0.943
_exptl_absorpt_coefficient_mu      0.413
_exptl_crystal_colour              ?
_exptl_crystal_density_diffrn      3.339
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         ?
_exptl_crystal_F_000               289
_exptl_crystal_size_max            0.145
_exptl_crystal_size_mid            0.127
_exptl_crystal_size_min            0.062
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0105
_diffrn_reflns_av_unetI/netI       0.0108
_diffrn_reflns_Laue_measured_fraction_full  0.516
_diffrn_reflns_Laue_measured_fraction_max  0.367
_diffrn_reflns_point_group_measured_fraction_full  0.516
_diffrn_reflns_point_group_measured_fraction_max  0.367
_diffrn_ambient_temperature        293(2)
_diffrn_detector_area_resol_mean   ?
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  165
_reflns_number_total               169
_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.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      ?
_refine_diff_density_max           0.402
_refine_diff_density_min           -0.391
_refine_diff_density_rms           0.119
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.300
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       42
_refine_ls_number_reflns           169
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0306
_refine_ls_R_factor_gt             0.0305
_refine_ls_restrained_S_all        1.300
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0564P)²+0.1418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0799
_refine_ls_wR_factor_ref           0.0802
_refine_special_details            ?
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
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
 M1A Fe+2 0.000000 0.000000 0.000000 0.0073(9) Uani 0.064(7) 2 d S . P . .
 M1B Mg+2 0.000000 0.000000 0.000000 0.0073(9) Uani 0.936(7) 2 d S . P . .
 M2A Fe+2 0.9898(3) 0.2777(2) 0.250000 0.0089(11) Uani 0.079(8) 2 d S T P . .
 M2B Mg+2 0.9898(3) 0.2777(2) 0.250000 0.0089(11) Uani 0.921(8) 2 d S T P . .
 Si Si+4 0.4267(3) 0.09404(18) 0.250000 0.0056(8) Uani 1 2 d S T P . .
 O1 O-2 0.7647(9) 0.0914(4) 0.250000 0.0081(12) Uani 1 2 d S T P . .
 O2 O-2 0.2194(7) 0.4474(4) 0.250000 0.0103(13) Uani 1 2 d S T P . .
 O3 O-2 0.2791(4) 0.1639(3) 0.0336(3) 0.0101(11) Uani 1 1 d . . . . .


_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
 M1A Si 2.6979(12) . ?
 M1A Si 2.6979(12) 5 ?
 M1A O1 2.088(3) 5_655 ?
 M1A O1 2.088(3) 1_455 ?
 M1A O2 2.076(2) 2_545 ?
 M1A O2 2.076(2) 6_565 ?
 M1A O3 2.142(3) . ?
 M1A O3 2.142(3) 5 ?
 M2A Si 2.796(2) 1_655 ?
 M2A O1 2.178(5) . ?
 M2A O2 2.044(4) 1_655 ?
 M2A O3 2.217(3) 7_656 ?
 M2A O3 2.217(3) 1_655 ?
 M2A O3 2.060(2) 6_666 ?
 M2A O3 2.060(2) 4 ?
 Si O1 1.608(4) . ?
 Si O2 1.647(4) 2_545 ?
 Si O3 1.636(2) . ?
 Si O3 1.636(2) 7_556 ?

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
 Si M1A Si 180.0 5 . ?
 O1 M1A Si 81.22(11) 5_655 5 ?
 O1 M1A Si 98.78(11) 1_455 5 ?
 O1 M1A Si 81.22(11) 1_455 . ?
 O1 M1A Si 98.78(11) 5_655 . ?
 O1 M1A O1 180.0(2) 5_655 1_455 ?
 O1 M1A O3 85.29(13) 5_655 5 ?
 O1 M1A O3 94.71(13) 1_455 5 ?
 O1 M1A O3 85.29(13) 1_455 . ?
 O1 M1A O3 94.71(13) 5_655 . ?
 O2 M1A Si 37.60(12) 6_565 5 ?
 O2 M1A Si 37.60(12) 2_545 . ?
 O2 M1A Si 142.40(12) 6_565 . ?
 O2 M1A Si 142.40(12) 2_545 5 ?
 O2 M1A O1 86.71(11) 6_565 5_655 ?
 O2 M1A O1 93.29(11) 6_565 1_455 ?
 O2 M1A O1 86.71(11) 2_545 1_455 ?
 O2 M1A O1 93.29(11) 2_545 5_655 ?
 O2 M1A O2 180.0(2) 6_565 2_545 ?
 O2 M1A O3 105.39(14) 6_565 . ?
 O2 M1A O3 74.61(14) 2_545 . ?
 O2 M1A O3 105.39(14) 2_545 5 ?
 O2 M1A O3 74.61(14) 6_565 5 ?
 O3 M1A Si 142.66(6) 5 . ?
 O3 M1A Si 142.66(6) . 5 ?
 O3 M1A Si 37.34(6) . . ?
 O3 M1A Si 37.34(6) 5 5 ?
 O3 M1A O3 180.0 5 . ?
 O1 M2A Si 77.47(13) . 1_655 ?
 O1 M2A O3 81.37(14) . 1_655 ?
 O1 M2A O3 81.37(14) . 7_656 ?
 O2 M2A Si 99.69(13) 1_655 1_655 ?
 O2 M2A O1 177.16(16) 1_655 . ?
 O2 M2A O3 96.33(13) 1_655 7_656 ?
 O2 M2A O3 90.89(13) 1_655 6_666 ?
 O2 M2A O3 90.89(13) 1_655 4 ?
 O2 M2A O3 96.33(13) 1_655 1_655 ?
 O3 M2A Si 123.71(8) 6_666 1_655 ?
 O3 M2A Si 123.71(8) 4 1_655 ?
 O3 M2A Si 35.80(6) 1_655 1_655 ?
 O3 M2A Si 35.80(6) 7_656 1_655 ?
 O3 M2A O1 90.72(11) 4 . ?
 O3 M2A O1 90.72(11) 6_666 . ?
 O3 M2A O3 159.21(11) 4 7_656 ?
 O3 M2A O3 159.21(11) 6_666 1_655 ?
 O3 M2A O3 71.52(11) 7_656 1_655 ?
 O3 M2A O3 88.35(7) 6_666 7_656 ?
 O3 M2A O3 111.07(15) 4 6_666 ?
 O3 M2A O3 88.35(7) 4 1_655 ?
 M1A Si M1A 67.41(3) . 3 ?
 M1A Si M2A 71.22(4) . 1_455 ?
 M1A Si M2A 71.22(4) 3 1_455 ?
 M1A Si M2B 74.91(4) . 2_645 ?
 M1A Si M2B 74.91(4) 3 2_645 ?
 M2A Si M2B 139.00(5) 1_455 2_645 ?
 O1 Si M1A 138.27(9) . 3 ?
 O1 Si M1A 138.27(9) . . ?
 O1 Si M2A 139.00(16) . 1_455 ?
 O1 Si M2B 82.00(16) . 2_645 ?
 O1 Si O2 113.99(19) . 2_545 ?
 O1 Si O3 115.87(11) . 7_556 ?
 O1 Si O3 115.87(11) . . ?
 O2 Si M1A 50.26(9) 2_545 3 ?
 O2 Si M1A 50.26(9) 2_545 . ?
 O2 Si M2A 107.02(13) 2_545 1_455 ?
 O2 Si M2B 31.98(12) 2_545 2_645 ?
 O3 Si M1A 105.71(10) 7_556 . ?
 O3 Si M1A 52.55(10) . . ?
 O3 Si M1A 105.71(10) . 3 ?
 O3 Si M1A 52.55(10) 7_556 3 ?
 O3 Si M2A 52.44(10) 7_556 1_455 ?
 O3 Si M2A 52.44(10) . 1_455 ?
 O3 Si M2B 118.93(12) . 2_645 ?
 O3 Si M2B 118.93(12) 7_556 2_645 ?
 O3 Si O2 102.29(14) . 2_545 ?
 O3 Si O2 102.29(14) 7_556 2_545 ?
 O3 Si O3 104.7(2) 7_556 . ?
 M1A O1 M1A 91.61(16) 3_655 1_655 ?
 M1A O1 M2A 97.15(15) 3_655 . ?
 M1A O1 M2A 97.15(15) 1_655 . ?
 Si O1 M1A 122.93(15) . 1_655 ?
 Si O1 M1A 122.93(15) . 3_655 ?
 Si O1 M2A 118.5(2) . . ?
 M1A O2 M1A 92.29(13) 2 4 ?
 M2A O2 M1A 124.17(13) 1_455 4 ?
 M2A O2 M1A 124.17(13) 1_455 2 ?
 Si O2 M1A 92.14(15) 2 2 ?
 Si O2 M1A 92.14(15) 2 4 ?
 Si O2 M2A 122.76(19) 2 1_455 ?
 M1A O3 M2A 94.43(10) . 1_455 ?
 M2A O3 M1A 116.70(11) 6_565 . ?
 M2A O3 M2A 129.25(14) 6_565 1_455 ?
 Si O3 M1A 90.11(14) . . ?
 Si O3 M2A 124.73(14) . 6_565 ?
 Si O3 M2A 91.75(9) . 1_455 ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 M1A Si O1 M1A -115.15(10) . . . 3_655 ?
 M1A Si O1 M1A 115.15(10) 3 . . 1_655 ?
 M1A Si O1 M1A -2.2(3) 3 . . 3_655 ?
 M1A Si O1 M1A 2.2(3) . . . 1_655 ?
 M1A Si O1 M2A -123.52(16) 3 . . . ?
 M1A Si O1 M2A 123.52(16) . . . . ?
 M1A Si O3 M1A -44.10(10) 3 . . . ?
 M1A Si O3 M2A 50.34(13) 3 . . 1_455 ?
 M1A Si O3 M2A 94.44(10) . . . 1_455 ?
 M1A Si O3 M2A -123.2(2) . . . 6_565 ?
 M1A Si O3 M2A -167.33(15) 3 . . 6_565 ?
 M2A Si O1 M1A -121.3(2) 1_455 . . 1_655 ?
 M2A Si O1 M1A 121.3(2) 1_455 . . 3_655 ?
 M2A Si O1 M2A 0.0 1_455 . . . ?
 M2A Si O3 M1A -94.44(10) 1_455 . . . ?
 M2A Si O3 M2A 142.3(2) 1_455 . . 6_565 ?
 M2B Si O1 M1A -58.7(2) 2_645 . . 3_655 ?
 M2B Si O1 M1A 58.7(2) 2_645 . . 1_655 ?
 M2B Si O1 M2A 180.0 2_645 . . . ?
 M2B Si O3 M1A 37.07(11) 2_645 . . . ?
 M2B Si O3 M2A 131.51(9) 2_645 . . 1_455 ?
 M2B Si O3 M2A -86.2(2) 2_645 . . 6_565 ?
 O1 Si O3 M1A 132.32(16) . . . . ?
 O1 Si O3 M2A -133.24(17) . . . 1_455 ?
 O1 Si O3 M2A 9.1(3) . . . 6_565 ?
 O2 Si O1 M1A 58.7(2) 2_545 . . 1_655 ?
 O2 Si O1 M1A -58.7(2) 2_545 . . 3_655 ?
 O2 Si O1 M2A 180.0 2_545 . . . ?
 O2 Si O3 M1A 7.70(13) 2_545 . . . ?
 O2 Si O3 M2A 102.14(13) 2_545 . . 1_455 ?
 O2 Si O3 M2A -115.5(2) 2_545 . . 6_565 ?
 O3 Si O1 M1A 59.7(3) 7_556 . . 3_655 ?
 O3 Si O1 M1A -177.02(19) . . . 3_655 ?
 O3 Si O1 M1A 177.02(19) 7_556 . . 1_655 ?
 O3 Si O1 M1A -59.7(3) . . . 1_655 ?
 O3 Si O1 M2A 61.66(16) . . . . ?
 O3 Si O1 M2A -61.66(16) 7_556 . . . ?
 O3 Si O3 M1A -98.71(16) 7_556 . . . ?
 O3 Si O3 M2A 138.06(13) 7_556 . . 6_565 ?
 O3 Si O3 M2A -4.3(2) 7_556 . . 1_455 ?


