 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'melanostibite'
_chemical_compound_source         'Sjogruvan, Sweden'
_chemical_formula_analytical
;      
Fe1.04 Mn1.96 Sb1.00 O6
;
_chemical_formula_sum
 'Fe Mn2 O6 Sb' 
_chemical_formula_weight          381.38

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'
 'Mn'  'Mn'   0.3368   0.7283
 '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'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            146
_space_group_name_H-M_alt         'R 3 :H'
_space_group_name_Hall            'R 3'
 
_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'
 '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'
 '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'
 
_cell_length_a                    5.2314(2)
_cell_length_b                    5.2314(2)
_cell_length_c                    14.3518(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      340.15(3)
_cell_formula_units_Z             3
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2347
_cell_measurement_theta_min       4.26
_cell_measurement_theta_max       32.52
 
_exptl_crystal_description        'anhedral'
_exptl_crystal_colour             'dark red'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     5.585          
_exptl_crystal_F_000              522.6
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.030
_exptl_crystal_size_mid           0.030
_exptl_crystal_size_min           0.015
_exptl_absorpt_coefficient_mu     14.327
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.655
_exptl_absorpt_correction_T_max   0.806
_exptl_absorpt_process_details    
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'microfocus'
_diffrn_measurement_device_type   'Bruker D8 Venture'
_diffrn_reflns_number             3082
_diffrn_reflns_av_unetI/netI      0.0223
_diffrn_reflns_av_R_equivalents   0.0296
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          4.260
_diffrn_reflns_theta_max          32.517
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              549
_reflns_number_gt                 549
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          1.000
_reflns_Friedel_fraction_max      1.000
_reflns_Friedel_fraction_full     1.000
 
_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      'Apex4 (Bruker AXS Inc., 2022)'
_computing_cell_refinement      'Apex4 (Bruker AXS Inc., 2022)'
_computing_data_reduction       'Apex4 (Bruker AXS Inc., 2022)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0142P)²] 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_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.92(6)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          549
_refine_ls_number_parameters      34
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0128
_refine_ls_R_factor_gt            0.0128
_refine_ls_wR_factor_ref          0.0286
_refine_ls_wR_factor_gt           0.0286
_refine_ls_goodness_of_fit_ref    1.055
_refine_ls_restrained_S_all       1.054
_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
M1FE Fe 0.000000 0.000000 0.18999(6) 0.0063(3) Uani 0.981(6) 3 d S T P . .
M1SB Sb 0.000000 0.000000 0.18999(6) 0.0063(3) Uani 0.019(6) 3 d S T P . .
M2 Mn 0.333333 0.666667 0.37094(7) 0.0078(3) Uani 1 3 d S T P . .
M3SB Sb 0.333333 0.666667 0.16086(2) 0.00509(11) Uani 0.949(8) 3 d S T P . .
M3FE Fe 0.333333 0.666667 0.16086(2) 0.00509(11) Uani 0.051(8) 3 d S T P . .
M4 Mn 0.000000 0.000000 0.97972(9) 0.0095(4) Uani 1 3 d S T P . .
O1 O 0.9812(6) 0.2891(8) 0.5838(2) 0.0076(6) Uani 1 1 d . . . . .
O2 O 0.2907(7) 0.3198(6) 0.09482(19) 0.0078(6) 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
M1FE O1 1.974(3) 8_544 ?
M1FE O1 1.974(3) 9_554 ?
M1FE O1 1.974(3) 7_444 ?
M1FE O2 2.105(3) 3 ?
M1FE O2 2.105(3) . ?
M1FE O2 2.105(3) 2 ?
M1FE M4 3.0178(15) 1_554 ?
M1FE M3SB 3.04914(17) 1_445 ?
M1FE M3SB 3.04916(17) . ?
M1FE M3SB 3.04918(17) 1_545 ?
M2 O2 2.100(3) 5 ?
M2 O2 2.100(3) 6_565 ?
M2 O2 2.100(3) 4_455 ?
M2 O1 2.331(4) 7_454 ?
M2 O1 2.331(4) 8_544 ?
M2 O1 2.331(4) 9_664 ?
M2 M3SB 3.0150(11) . ?
M2 M4 3.1325(4) 4_554 ?
M2 M4 3.1325(4) 4_454 ?
M2 M4 3.1325(4) 4_564 ?
M3SB O2 1.958(3) 2_665 ?
M3SB O2 1.958(3) . ?
M3SB O2 1.958(3) 3_565 ?
M3SB O1 2.025(3) 7_454 ?
M3SB O1 2.025(3) 8_544 ?
M3SB O1 2.025(3) 9_664 ?
M4 O1 2.112(3) 4_345 ?
M4 O1 2.112(3) 6_565 ?
M4 O1 2.112(3) 5_545 ?
M4 O2 2.301(3) 3_556 ?
M4 O2 2.301(3) 1_556 ?
M4 O2 2.301(3) 2_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
O1 M1FE O1 102.11(10) 8_544 9_554 ?
O1 M1FE O1 102.11(10) 8_544 7_444 ?
O1 M1FE O1 102.11(10) 9_554 7_444 ?
O1 M1FE O2 162.89(13) 8_544 3 ?
O1 M1FE O2 93.75(10) 9_554 3 ?
O1 M1FE O2 80.50(9) 7_444 3 ?
O1 M1FE O2 80.50(9) 8_544 . ?
O1 M1FE O2 162.89(13) 9_554 . ?
O1 M1FE O2 93.75(10) 7_444 . ?
O2 M1FE O2 82.46(13) 3 . ?
O1 M1FE O2 93.75(10) 8_544 2 ?
O1 M1FE O2 80.50(9) 9_554 2 ?
O1 M1FE O2 162.89(13) 7_444 2 ?
O2 M1FE O2 82.46(13) 3 2 ?
O2 M1FE O2 82.46(13) . 2 ?
O1 M1FE M4 116.10(8) 8_544 1_554 ?
O1 M1FE M4 116.10(8) 9_554 1_554 ?
O1 M1FE M4 116.10(8) 7_444 1_554 ?
O2 M1FE M4 49.55(9) 3 1_554 ?
O2 M1FE M4 49.55(9) . 1_554 ?
O2 M1FE M4 49.56(9) 2 1_554 ?
O1 M1FE M3SB 99.26(10) 8_544 1_445 ?
O1 M1FE M3SB 40.94(9) 9_554 1_445 ?
O1 M1FE M3SB 140.84(10) 7_444 1_445 ?
O2 M1FE M3SB 88.46(9) 3 1_445 ?
O2 M1FE M3SB 122.05(10) . 1_445 ?
O2 M1FE M3SB 39.59(8) 2 1_445 ?
M4 M1FE M3SB 82.118(16) 1_554 1_445 ?
O1 M1FE M3SB 40.94(9) 8_544 . ?
O1 M1FE M3SB 140.85(10) 9_554 . ?
O1 M1FE M3SB 99.26(10) 7_444 . ?
O2 M1FE M3SB 122.05(10) 3 . ?
O2 M1FE M3SB 39.59(8) . . ?
O2 M1FE M3SB 88.46(9) 2 . ?
M4 M1FE M3SB 82.118(16) 1_554 . ?
M3SB M1FE M3SB 118.151(8) 1_445 . ?
O1 M1FE M3SB 140.84(10) 8_544 1_545 ?
O1 M1FE M3SB 99.26(10) 9_554 1_545 ?
O1 M1FE M3SB 40.93(9) 7_444 1_545 ?
O2 M1FE M3SB 39.59(8) 3 1_545 ?
O2 M1FE M3SB 88.46(9) . 1_545 ?
O2 M1FE M3SB 122.05(10) 2 1_545 ?
M4 M1FE M3SB 82.118(16) 1_554 1_545 ?
M3SB M1FE M3SB 118.150(8) 1_445 1_545 ?
M3SB M1FE M3SB 118.151(8) . 1_545 ?
O2 M2 O2 105.70(10) 5 6_565 ?
O2 M2 O2 105.70(10) 5 4_455 ?
O2 M2 O2 105.70(10) 6_565 4_455 ?
O2 M2 O1 155.13(13) 5 7_454 ?
O2 M2 O1 89.63(10) 6_565 7_454 ?
O2 M2 O1 88.24(10) 4_455 7_454 ?
O2 M2 O1 88.24(10) 5 8_544 ?
O2 M2 O1 155.13(13) 6_565 8_544 ?
O2 M2 O1 89.63(10) 4_455 8_544 ?
O1 M2 O1 71.04(13) 7_454 8_544 ?
O2 M2 O1 89.63(10) 5 9_664 ?
O2 M2 O1 88.24(10) 6_565 9_664 ?
O2 M2 O1 155.13(13) 4_455 9_664 ?
O1 M2 O1 71.04(13) 7_454 9_664 ?
O1 M2 O1 71.04(12) 8_544 9_664 ?
O2 M2 M3SB 113.02(9) 5 . ?
O2 M2 M3SB 113.02(9) 6_565 . ?
O2 M2 M3SB 113.02(9) 4_455 . ?
O1 M2 M3SB 42.13(8) 7_454 . ?
O1 M2 M3SB 42.13(8) 8_544 . ?
O1 M2 M3SB 42.13(8) 9_664 . ?
O2 M2 M4 47.28(9) 5 4_554 ?
O2 M2 M4 97.58(7) 6_565 4_554 ?
O2 M2 M4 149.07(7) 4_455 4_554 ?
O1 M2 M4 112.35(8) 7_454 4_554 ?
O1 M2 M4 76.59(8) 8_544 4_554 ?
O1 M2 M4 42.40(8) 9_664 4_554 ?
M3SB M2 M4 74.62(2) . 4_554 ?
O2 M2 M4 97.58(7) 5 4_454 ?
O2 M2 M4 149.07(7) 6_565 4_454 ?
O2 M2 M4 47.28(9) 4_455 4_454 ?
O1 M2 M4 76.59(8) 7_454 4_454 ?
O1 M2 M4 42.41(8) 8_544 4_454 ?
O1 M2 M4 112.35(8) 9_664 4_454 ?
M3SB M2 M4 74.62(2) . 4_454 ?
M4 M2 M4 113.236(19) 4_554 4_454 ?
O2 M2 M4 149.07(7) 5 4_564 ?
O2 M2 M4 47.28(9) 6_565 4_564 ?
O2 M2 M4 97.58(7) 4_455 4_564 ?
O1 M2 M4 42.40(8) 7_454 4_564 ?
O1 M2 M4 112.35(8) 8_544 4_564 ?
O1 M2 M4 76.60(8) 9_664 4_564 ?
M3SB M2 M4 74.62(2) . 4_564 ?
M4 M2 M4 113.236(19) 4_554 4_564 ?
M4 M2 M4 113.235(19) 4_454 4_564 ?
O2 M3SB O2 98.56(10) 2_665 . ?
O2 M3SB O2 98.55(10) 2_665 3_565 ?
O2 M3SB O2 98.56(10) . 3_565 ?
O2 M3SB O1 94.12(11) 2_665 7_454 ?
O2 M3SB O1 166.85(11) . 7_454 ?
O2 M3SB O1 82.92(12) 3_565 7_454 ?
O2 M3SB O1 166.85(11) 2_665 8_544 ?
O2 M3SB O1 82.92(12) . 8_544 ?
O2 M3SB O1 94.12(11) 3_565 8_544 ?
O1 M3SB O1 83.95(15) 7_454 8_544 ?
O2 M3SB O1 82.92(12) 2_665 9_664 ?
O2 M3SB O1 94.12(11) . 9_664 ?
O2 M3SB O1 166.85(11) 3_565 9_664 ?
O1 M3SB O1 83.94(15) 7_454 9_664 ?
O1 M3SB O1 83.94(15) 8_544 9_664 ?
O2 M3SB M2 118.94(8) 2_665 . ?
O2 M3SB M2 118.94(8) . . ?
O2 M3SB M2 118.94(8) 3_565 . ?
O1 M3SB M2 50.55(10) 7_454 . ?
O1 M3SB M2 50.55(10) 8_544 . ?
O1 M3SB M2 50.56(10) 9_664 . ?
O2 M3SB M1FE 139.77(10) 2_665 . ?
O2 M3SB M1FE 43.24(8) . . ?
O2 M3SB M1FE 99.45(10) 3_565 . ?
O1 M3SB M1FE 123.61(9) 7_454 . ?
O1 M3SB M1FE 39.70(9) 8_544 . ?
O1 M3SB M1FE 87.39(9) 9_664 . ?
M2 M3SB M1FE 82.118(16) . . ?
O2 M3SB M1FE 99.45(10) 2_665 1_565 ?
O2 M3SB M1FE 139.77(10) . 1_565 ?
O2 M3SB M1FE 43.24(8) 3_565 1_565 ?
O1 M3SB M1FE 39.70(9) 7_454 1_565 ?
O1 M3SB M1FE 87.39(8) 8_544 1_565 ?
O1 M3SB M1FE 123.61(9) 9_664 1_565 ?
M2 M3SB M1FE 82.117(16) . 1_565 ?
M1FE M3SB M1FE 118.151(8) . 1_565 ?
O2 M3SB M1FE 43.24(8) 2_665 1_665 ?
O2 M3SB M1FE 99.45(10) . 1_665 ?
O2 M3SB M1FE 139.77(10) 3_565 1_665 ?
O1 M3SB M1FE 87.39(8) 7_454 1_665 ?
O1 M3SB M1FE 123.61(9) 8_544 1_665 ?
O1 M3SB M1FE 39.70(9) 9_664 1_665 ?
M2 M3SB M1FE 82.117(16) . 1_665 ?
M1FE M3SB M1FE 118.151(8) . 1_665 ?
M1FE M3SB M1FE 118.150(8) 1_565 1_665 ?
O1 M4 O1 103.24(10) 4_345 6_565 ?
O1 M4 O1 103.24(10) 4_345 5_545 ?
O1 M4 O1 103.24(10) 6_565 5_545 ?
O1 M4 O2 90.12(15) 4_345 3_556 ?
O1 M4 O2 159.25(11) 6_565 3_556 ?
O1 M4 O2 88.74(10) 5_545 3_556 ?
O1 M4 O2 159.25(11) 4_345 1_556 ?
O1 M4 O2 88.74(10) 6_565 1_556 ?
O1 M4 O2 90.12(15) 5_545 1_556 ?
O2 M4 O2 74.16(10) 3_556 1_556 ?
O1 M4 O2 88.74(10) 4_345 2_556 ?
O1 M4 O2 90.12(15) 6_565 2_556 ?
O1 M4 O2 159.25(11) 5_545 2_556 ?
O2 M4 O2 74.16(10) 3_556 2_556 ?
O2 M4 O2 74.16(10) 1_556 2_556 ?
O1 M4 M1FE 115.15(9) 4_345 1_556 ?
O1 M4 M1FE 115.15(9) 6_565 1_556 ?
O1 M4 M1FE 115.15(9) 5_545 1_556 ?
O2 M4 M1FE 44.12(7) 3_556 1_556 ?
O2 M4 M1FE 44.12(7) 1_556 1_556 ?
O2 M4 M1FE 44.13(7) 2_556 1_556 ?
O1 M4 M2 99.52(8) 4_345 7_445 ?
O1 M4 M2 48.08(10) 6_565 7_445 ?
O1 M4 M2 147.23(9) 5_545 7_445 ?
O2 M4 M2 114.63(7) 3_556 7_445 ?
O2 M4 M2 75.78(9) 1_556 7_445 ?
O2 M4 M2 42.09(8) 2_556 7_445 ?
M1FE M4 M2 74.62(2) 1_556 7_445 ?
O1 M4 M2 147.23(9) 4_345 7_545 ?
O1 M4 M2 99.52(9) 6_565 7_545 ?
O1 M4 M2 48.07(10) 5_545 7_545 ?
O2 M4 M2 75.78(9) 3_556 7_545 ?
O2 M4 M2 42.09(8) 1_556 7_545 ?
O2 M4 M2 114.63(7) 2_556 7_545 ?
M1FE M4 M2 74.62(2) 1_556 7_545 ?
M2 M4 M2 113.237(19) 7_445 7_545 ?
O1 M4 M2 48.08(10) 4_345 7_435 ?
O1 M4 M2 147.23(9) 6_565 7_435 ?
O1 M4 M2 99.52(9) 5_545 7_435 ?
O2 M4 M2 42.09(9) 3_556 7_435 ?
O2 M4 M2 114.63(7) 1_556 7_435 ?
O2 M4 M2 75.78(9) 2_556 7_435 ?
M1FE M4 M2 74.62(2) 1_556 7_435 ?
M2 M4 M2 113.237(19) 7_445 7_435 ?
M2 M4 M2 113.235(19) 7_545 7_435 ?
M1FE O1 M3SB 99.36(14) 4 4_545 ?
M1FE O1 M4 117.74(17) 4 7_654 ?
M3SB O1 M4 128.55(14) 4_545 7_654 ?
M1FE O1 M2 135.26(14) 4 4_545 ?
M3SB O1 M2 87.31(13) 4_545 4_545 ?
M4 O1 M2 89.52(12) 7_654 4_545 ?
M3SB O2 M2 119.15(15) . 7_544 ?
M3SB O2 M1FE 97.17(12) . . ?
M2 O2 M1FE 124.94(14) 7_544 . ?
M3SB O2 M4 138.48(17) . 1_554 ?
M2 O2 M4 90.63(12) 7_544 1_554 ?
M1FE O2 M4 86.32(11) . 1_554 ?
 
_refine_diff_density_max    0.558
_refine_diff_density_min   -0.606
_refine_diff_density_rms    0.145



