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#$Date: 2024-02-04 14:20:56 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289584 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/29/7062929.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_7062929
loop_
_publ_author_name
'Shvanskaya, Larisa V.'
'Krikunova, Polina V.'
'Vasilchikova, Tatyana M.'
'Borovikova, Elena Y.'
'Volkova, Olga S.'
'Vasiliev, Alexander N.'
_publ_section_title
;
 Crystal structure, infrared spectroscopy and thermodynamic properties of
 a manganese member of the ellenbergerite family
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1952
_journal_page_last               1957
_journal_paper_doi               10.1039/D3NJ05142K
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'H7 Mn13.50 O37.69 V8, 1.392(H)'
_chemical_formula_sum            'H4.2 Mn6.75 O18.845 V4'
_chemical_formula_weight         880.335
_chemical_name_common            'Manganese hydroxide vanadate divanadate'
_chemical_name_systematic
'Hexamanganese manganese trihydroxide dihydrogen/hydrogenvanadate divanadate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.1893(5)
_cell_length_b                   13.1893(5)
_cell_length_c                   5.2408(2)
_cell_measurement_reflns_used    7817
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.502
_cell_volume                     789.54(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7817
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_min         3.089
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_T_max  0.6501
_exptl_absorpt_correction_T_min  0.5105
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            black
_exptl_crystal_density_diffrn    3.706
_exptl_crystal_description       needle
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         858
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0180
_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)+(0.0171P)²+0.2347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0400
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                816
_reflns_number_total             858
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj05142k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7062929.cif.'
_cod_original_cell_volume        789.54(7)
_cod_original_formula_sum        'H4.20 Mn6.75 O18.845 V4'
_cod_database_code               7062929
_shelx_shelxl_version_number     2018/3
_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, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
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
Mn1 Mn 0.42652(4) 0.34748(4) -0.02641(7) 0.00622(13) Uani 1 1 d . . . . .
Mn2 Mn 0.000000 0.000000 0.1493(4) 0.0174(6) Uani 0.749(5) 6 d S T . . .
V1 V 0.30128(6) 0.15064(3) 0.44837(16) 0.00590(17) Uani 1 2 d S T P . .
V2A V 0.666667 0.333333 -0.2884(3) 0.0066(3) Uani 0.847(3) 6 d S T P . .
V2B V 0.666667 0.333333 -0.007(2) 0.0066(3) Uani 0.153(3) 6 d S T P . .
O1 O 0.1524(3) 0.07621(14) 0.4001(7) 0.0126(7) Uani 1 2 d S T P . .
O2 O 0.3795(3) 0.18977(15) 0.1644(6) 0.0083(6) Uani 1 2 d S T P . .
O3 O 0.3420(2) 0.2747(2) 0.6222(5) 0.0084(5) Uani 1 1 d . . . . .
O4 O 0.52559(15) 0.47441(15) 0.2851(6) 0.0083(7) Uani 1 2 d DS T P . .
O5 O 0.59648(17) 0.40352(17) -0.1762(10) 0.0234(10) Uani 1 2 d DS T P . .
O6 O 0.666667 0.333333 0.375(2) 0.044(3) Uani 0.847(3) 6 d DS T P . .
H1 H 0.5566(16) 0.4434(16) 0.394(9) 0.009(13) Uiso 1 2 d DS . P . .
H2 H 0.626613 0.373(13) 0.41(2) 0.009(13) Uiso 0.232 2 d DS . P . .
H3 H 0.610(13) 0.390(13) -0.01(2) 0.009(13) Uiso 0.168 2 d DS . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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 O3 89.16(10) . 10_554 ?
O2 Mn1 O3 97.88(11) . 1_554 ?
O3 Mn1 O3 91.70(9) 10_554 1_554 ?
O2 Mn1 O5 104.90(14) . . ?
O3 Mn1 O5 164.16(11) 10_554 . ?
O3 Mn1 O5 93.51(14) 1_554 . ?
O2 Mn1 O4 99.58(12) . . ?
O3 Mn1 O4 86.88(10) 10_554 . ?
O3 Mn1 O4 162.46(10) 1_554 . ?
O5 Mn1 O4 83.65(13) . . ?
O2 Mn1 O4 176.36(12) . 4_664 ?
O3 Mn1 O4 88.02(10) 10_554 4_664 ?
O3 Mn1 O4 84.50(9) 1_554 4_664 ?
O5 Mn1 O4 77.62(13) . 4_664 ?
O4 Mn1 O4 77.98(6) . 4_664 ?
O2 Mn1 Mn1 129.94(10) . 7_665 ?
O3 Mn1 Mn1 119.37(6) 10_554 7_665 ?
O3 Mn1 Mn1 119.34(6) 1_554 7_665 ?
O5 Mn1 Mn1 45.56(8) . 7_665 ?
O4 Mn1 Mn1 48.14(6) . 7_665 ?
O4 Mn1 Mn1 50.15(6) 4_664 7_665 ?
O2 Mn1 Mn1 87.12(8) . 10 ?
O3 Mn1 Mn1 41.30(7) 10_554 10 ?
O3 Mn1 Mn1 132.84(7) 1_554 10 ?
O5 Mn1 Mn1 130.58(11) . 10 ?
O4 Mn1 Mn1 46.94(7) . 10 ?
O4 Mn1 Mn1 89.24(8) 4_664 10 ?
Mn1 Mn1 Mn1 90.0 7_665 10 ?
O2 Mn1 Mn1 137.13(10) . 10_554 ?
O3 Mn1 Mn1 81.65(7) 10_554 10_554 ?
O3 Mn1 Mn1 41.24(6) 1_554 10_554 ?
O5 Mn1 Mn1 92.48(14) . 10_554 ?
O4 Mn1 Mn1 121.41(8) . 10_554 ?
O4 Mn1 Mn1 44.56(6) 4_664 10_554 ?
Mn1 Mn1 Mn1 90.0 7_665 10_554 ?
Mn1 Mn1 Mn1 110.86(3) 10 10_554 ?
O1 Mn2 O1 87.71(15) 4_554 5_554 ?
O1 Mn2 O1 87.71(15) 4_554 6_554 ?
O1 Mn2 O1 87.71(15) 5_554 6_554 ?
O1 Mn2 O1 179.81(18) 4_554 . ?
O1 Mn2 O1 92.43(7) 5_554 . ?
O1 Mn2 O1 92.43(7) 6_554 . ?
O1 Mn2 O1 92.43(7) 4_554 2 ?
O1 Mn2 O1 179.81(18) 5_554 2 ?
O1 Mn2 O1 92.43(7) 6_554 2 ?
O1 Mn2 O1 87.44(15) . 2 ?
O1 Mn2 O1 92.43(7) 4_554 3 ?
O1 Mn2 O1 92.43(7) 5_554 3 ?
O1 Mn2 O1 179.81(18) 6_554 3 ?
O1 Mn2 O1 87.44(15) . 3 ?
O1 Mn2 O1 87.44(15) 2 3 ?
O1 Mn2 Mn2 53.13(10) 4_554 4_554 ?
O1 Mn2 Mn2 53.13(10) 5_554 4_554 ?
O1 Mn2 Mn2 53.13(10) 6_554 4_554 ?
O1 Mn2 Mn2 127.06(10) . 4_554 ?
O1 Mn2 Mn2 127.06(10) 2 4_554 ?
O1 Mn2 Mn2 127.06(10) 3 4_554 ?
O1 Mn2 Mn2 126.87(10) 4_554 4 ?
O1 Mn2 Mn2 126.87(10) 5_554 4 ?
O1 Mn2 Mn2 126.87(10) 6_554 4 ?
O1 Mn2 Mn2 52.94(10) . 4 ?
O1 Mn2 Mn2 52.94(10) 2 4 ?
O1 Mn2 Mn2 52.94(10) 3 4 ?
Mn2 Mn2 Mn2 180.0 4_554 4 ?
O3 V1 O3 106.42(16) 9 . ?
O3 V1 O1 110.34(11) 9 . ?
O3 V1 O1 110.34(11) . . ?
O3 V1 O2 108.49(10) 9 . ?
O3 V1 O2 108.49(10) . . ?
O1 V1 O2 112.54(17) . . ?
V2B V2A O5 69.85(18) . . ?
V2B V2A O5 69.85(18) . 3_665 ?
O5 V2A O5 108.78(19) . 3_665 ?
V2B V2A O5 69.85(18) . 2_655 ?
O5 V2A O5 108.78(19) . 2_655 ?
O5 V2A O5 108.78(19) 3_665 2_655 ?
V2B V2A O6 180.0 . 1_554 ?
O5 V2A O6 110.15(19) . 1_554 ?
O5 V2A O6 110.15(19) 3_665 1_554 ?
O5 V2A O6 110.15(19) 2_655 1_554 ?
V2B V2A H3 42(5) . . ?
O5 V2A H3 28(4) . . ?
O5 V2A H3 93(3) 3_665 . ?
O5 V2A H3 93(3) 2_655 . ?
O6 V2A H3 138(5) 1_554 . ?
V2B V2A H3 42(4) . 2_655 ?
O5 V2A H3 93(3) . 2_655 ?
O5 V2A H3 93(3) 3_665 2_655 ?
O5 V2A H3 28(4) 2_655 2_655 ?
O6 V2A H3 138(4) 1_554 2_655 ?
H3 V2A H3 70(7) . 2_655 ?
V2B V2A H3 42(5) . 3_665 ?
O5 V2A H3 93(3) . 3_665 ?
O5 V2A H3 28(4) 3_665 3_665 ?
O5 V2A H3 93(3) 2_655 3_665 ?
O6 V2A H3 138(4) 1_554 3_665 ?
H3 V2A H3 70(7) . 3_665 ?
H3 V2A H3 70(7) 2_655 3_665 ?
V2A V2B O5 61.1(3) . . ?
V2A V2B O5 61.1(3) . 2_655 ?
O5 V2B O5 98.6(4) . 2_655 ?
V2A V2B O5 61.1(3) . 3_665 ?
O5 V2B O5 98.6(4) . 3_665 ?
O5 V2B O5 98.6(4) 2_655 3_665 ?
V2A V2B O6 180.0 . . ?
O5 V2B O6 118.9(3) . . ?
O5 V2B O6 118.9(3) 2_655 . ?
O5 V2B O6 118.9(3) 3_665 . ?
V2A V2B H3 89(5) . . ?
O5 V2B H3 28(5) . . ?
O5 V2B H3 115(3) 2_655 . ?
O5 V2B H3 115(3) 3_665 . ?
O6 V2B H3 91(5) . . ?
V2A V2B H3 89(5) . 2_655 ?
O5 V2B H3 115(3) . 2_655 ?
O5 V2B H3 28(5) 2_655 2_655 ?
O5 V2B H3 115(3) 3_665 2_655 ?
O6 V2B H3 91(5) . 2_655 ?
H3 V2B H3 120.0(4) . 2_655 ?
V2A V2B H3 89(5) . 3_665 ?
O5 V2B H3 115(3) . 3_665 ?
O5 V2B H3 115(3) 2_655 3_665 ?
O5 V2B H3 28(5) 3_665 3_665 ?
O6 V2B H3 91(5) . 3_665 ?
H3 V2B H3 120.0(4) . 3_665 ?
H3 V2B H3 120.0(4) 2_655 3_665 ?
V1 O1 Mn2 134.7(2) . 4 ?
V1 O1 Mn2 151.4(2) . . ?
Mn2 O1 Mn2 73.93(10) 4 . ?
V1 O2 Mn1 122.62(8) . 9 ?
V1 O2 Mn1 122.62(8) . . ?
Mn1 O2 Mn1 114.67(16) 9 . ?
V1 O3 Mn1 123.78(13) . 10 ?
V1 O3 Mn1 137.74(13) . 1_556 ?
Mn1 O3 Mn1 97.46(10) 10 1_556 ?
Mn1 O4 Mn1 83.72(11) . 7_665 ?
Mn1 O4 Mn1 146.02(16) . 4_665 ?
Mn1 O4 Mn1 88.51(5) 7_665 4_665 ?
Mn1 O4 Mn1 88.51(5) . 10 ?
Mn1 O4 Mn1 146.01(16) 7_665 10 ?
Mn1 O4 Mn1 79.71(11) 4_665 10 ?
Mn1 O4 H1 110(2) . . ?
Mn1 O4 H1 110(2) 7_665 . ?
Mn1 O4 H1 103(3) 4_665 . ?
Mn1 O4 H1 103(3) 10 . ?
V2A O5 V2B 49.0(3) . . ?
V2A O5 Mn1 134.50(9) . . ?
V2B O5 Mn1 110.9(3) . . ?
V2A O5 Mn1 134.50(9) . 7_665 ?
V2B O5 Mn1 110.9(3) . 7_665 ?
Mn1 O5 Mn1 88.89(15) . 7_665 ?
V2A O5 H3 90(10) . . ?
V2B O5 H3 41(10) . . ?
Mn1 O5 H3 82(10) . . ?
Mn1 O5 H3 82(10) 7_665 . ?
V2A O6 V2B 180.0 1_556 . ?
V2A O6 H2 80(7) 1_556 . ?
V2B O6 H2 100(7) . . ?
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 2.1028(18) . ?
Mn1 O3 2.116(2) 10_554 ?
Mn1 O3 2.118(2) 1_554 ?
Mn1 O5 2.129(3) . ?
Mn1 O4 2.233(2) . ?
Mn1 O4 2.326(3) 4_664 ?
Mn1 Mn1 2.9808(8) 7_665 ?
Mn1 Mn1 3.1823(5) 10 ?
Mn1 Mn1 3.1823(5) 10_554 ?
Mn2 O1 2.176(4) 4_554 ?
Mn2 O1 2.176(4) 5_554 ?
Mn2 O1 2.176(4) 6_554 ?
Mn2 O1 2.182(4) . ?
Mn2 O1 2.182(4) 2 ?
Mn2 O1 2.182(4) 3 ?
Mn2 Mn2 2.62038(10) 4_554 ?
Mn2 Mn2 2.62042(10) 4 ?
V1 O3 1.708(2) 9 ?
V1 O3 1.708(2) . ?
V1 O1 1.719(3) . ?
V1 O2 1.736(3) . ?
V2A V2B 1.473(11) . ?
V2A O5 1.708(4) . ?
V2A O5 1.708(4) 3_665 ?
V2A O5 1.708(4) 2_655 ?
V2A O6 1.763(13) 1_554 ?
V2A H3 1.9(3) . ?
V2A H3 1.9(3) 2_655 ?
V2A H3 1.9(3) 3_665 ?
V2B O5 1.831(7) . ?
V2B O5 1.831(7) 2_655 ?
V2B O5 1.831(7) 3_665 ?
V2B O6 2.005(18) . ?
V2B H3 1.3(3) . ?
V2B H3 1.3(3) 2_655 ?
V2B H3 1.3(3) 3_665 ?
O4 H1 0.911(14) . ?
O5 H3 0.918(15) . ?
O6 H2 0.93(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H1 O5 0.911(14) 2.43(3) 3.255(6) 151(5) 1_556 yes
O4 H1 O6 0.911(14) 2.52(4) 3.257(4) 139(4) . yes
O6 H2 O4 0.93(2) 2.39(3) 3.257(4) 155(10) . yes
O6 H2 O5 0.93(2) 2.30(12) 2.846(11) 117(8) 1_556 yes
O5 H3 O6 0.918(15) 2.40(7) 3.304(12) 168(28) . yes
