#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012733.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7012733
loop_
_publ_author_name
'Irvine, John T. S.'
'Johnston, Magnus G.'
'Harrison, William T. A.'
_publ_section_title
;
 Lone-pair containment in closed cavities. The MTe6O13 (M = Mn, Ni, Co)
 family of ternary oxides
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2641
_journal_paper_doi               10.1039/b300573a
_journal_year                    2003
_chemical_formula_sum            'Mn O13 Te6'
_chemical_formula_weight         1028.54
_chemical_melting_point          'decomposes before melting'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.2505(5)
_cell_length_b                   10.2505(5)
_cell_length_c                   19.2195(9)
_cell_measurement_reflns_used    4318
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.48
_cell_measurement_theta_min      3.21
_cell_volume                     1748.89(15)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5886
_diffrn_reflns_theta_full        32.49
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    15.920
_exptl_absorpt_correction_T_max  0.251
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'very pale pink'
_exptl_crystal_density_diffrn    5.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'faceted rhomb'
_exptl_crystal_F_000             2646
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       0.00066(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0171P)²+16.2711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                1360
_reflns_number_total             1417
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b300573a.txt
_cod_data_source_block           mto
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7012733
loop_
_symmetry_equiv_pos_as_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'
'-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'
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
Mn1 Mn 0.0000 0.0000 0.24417(4) 0.00862(16) Uani 1 3 d S . .
Te1 Te 0.15413(3) 0.23722(3) 0.404036(11) 0.00994(7) Uani 1 1 d . . .
Te2 Te 0.23094(2) 0.05956(3) 0.091045(11) 0.00858(7) Uani 1 1 d . . .
O1 O 0.0876(3) 0.2059(3) 0.30814(13) 0.0142(5) Uani 1 1 d . . .
O2 O 0.1968(3) 0.0486(3) 0.18604(13) 0.0131(5) Uani 1 1 d . . .
O3 O 0.0000 0.0000 0.4113(2) 0.0115(8) Uani 1 3 d S . .
O4 O 0.3335(3) -0.0819(3) 0.11389(14) 0.0141(5) Uani 1 1 d . . .
O5 O 0.1289(3) 0.1822(3) 0.06988(14) 0.0128(5) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0084(2) 0.0084(2) 0.0091(4) 0.000 0.000 0.00420(12)
Te1 0.00907(11) 0.01306(11) 0.00962(11) -0.00099(7) -0.00017(7) 0.00697(8)
Te2 0.00792(10) 0.00924(11) 0.00818(10) 0.00038(6) 0.00084(6) 0.00400(8)
O1 0.0212(13) 0.0089(11) 0.0104(10) -0.0009(8) -0.0031(9) 0.0058(10)
O2 0.0115(11) 0.0185(13) 0.0098(11) 0.0017(9) 0.0020(9) 0.0078(10)
O3 0.0091(11) 0.0091(11) 0.016(2) 0.000 0.000 0.0046(6)
O4 0.0141(12) 0.0158(12) 0.0167(12) 0.0016(9) 0.0040(9) 0.0106(10)
O5 0.0103(11) 0.0132(11) 0.0164(12) 0.0001(9) 0.0004(9) 0.0072(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 Mn1 O2 95.14(10) 3 2 ?
O2 Mn1 O2 95.14(10) 3 . ?
O2 Mn1 O2 95.14(10) 2 . ?
O2 Mn1 O1 162.05(11) 3 . ?
O2 Mn1 O1 74.90(10) 2 . ?
O2 Mn1 O1 100.54(11) . . ?
O2 Mn1 O1 100.54(11) 3 3 ?
O2 Mn1 O1 162.05(11) 2 3 ?
O2 Mn1 O1 74.90(10) . 3 ?
O1 Mn1 O1 92.01(10) . 3 ?
O2 Mn1 O1 74.90(10) 3 2 ?
O2 Mn1 O1 100.54(11) 2 2 ?
O2 Mn1 O1 162.05(11) . 2 ?
O1 Mn1 O1 92.01(10) . 2 ?
O1 Mn1 O1 92.01(10) 3 2 ?
O4 Te1 O1 101.33(12) 4_455 . ?
O4 Te1 O3 83.47(10) 4_455 . ?
O1 Te1 O3 82.81(14) . . ?
O4 Te1 O1 91.90(12) 4_455 16 ?
O1 Te1 O1 73.92(12) . 16 ?
O3 Te1 O1 154.92(12) . 16 ?
O4 Te1 Te1 97.90(8) 4_455 16 ?
O1 Te1 Te1 39.51(8) . 16 ?
O3 Te1 Te1 121.74(11) . 16 ?
O1 Te1 Te1 34.41(7) 16 16 ?
O2 Te2 O5 95.31(12) . 3 ?
O2 Te2 O5 95.42(11) . . ?
O5 Te2 O5 93.29(15) 3 . ?
O2 Te2 O4 84.38(11) . . ?
O5 Te2 O4 84.56(11) 3 . ?
O5 Te2 O4 177.81(10) . . ?
O2 Te2 O2 73.20(11) . 13 ?
O5 Te2 O2 166.59(10) 3 13 ?
O5 Te2 O2 94.65(10) . 13 ?
O4 Te2 O2 87.39(10) . 13 ?
Te1 O1 Te1 106.08(12) . 16 ?
Te1 O1 Mn1 129.05(13) . . ?
Te1 O1 Mn1 122.49(12) 16 . ?
Te2 O2 Mn1 131.11(14) . . ?
Te2 O2 Te2 106.80(11) . 13 ?
Mn1 O2 Te2 110.38(11) . 13 ?
Te1 O3 Te1 119.58(3) 2 . ?
Te1 O3 Te1 119.58(3) 2 3 ?
Te1 O3 Te1 119.58(3) . 3 ?
Te1 O4 Te2 131.56(14) 7_544 . ?
Te2 O5 Te2 137.13(14) 2 . ?
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
Mn1 O2 2.136(3) 3 ?
Mn1 O2 2.136(3) 2 ?
Mn1 O2 2.136(3) . ?
Mn1 O1 2.208(3) . ?
Mn1 O1 2.208(3) 3 ?
Mn1 O1 2.208(3) 2 ?
Te1 O4 1.853(3) 4_455 ?
Te1 O1 1.936(3) . ?
Te1 O3 2.1416(4) . ?
Te1 O1 2.179(3) 16 ?
Te1 Te1 3.2907(5) 16 ?
Te2 O2 1.852(3) . ?
Te2 O5 1.922(3) 3 ?
Te2 O5 2.039(3) . ?
Te2 O4 2.219(3) . ?
Te2 O2 2.615(3) 13 ?
O1 Te1 2.179(3) 16 ?
O2 Te2 2.615(3) 13 ?
O3 Te1 2.1416(4) 2 ?
O3 Te1 2.1416(4) 3 ?
O4 Te1 1.853(3) 7_544 ?
O5 Te2 1.922(3) 2 ?
