Crystal structure, infrared spectroscopy and thermodynamic properties of a manganese member of the ellenbergerite family
Shvanskaya, Larisa V.; Krikunova, Polina V.; Vasilchikova, Tatyana M.; Borovikova, Elena Y.; Volkova, Olga S.; Vasiliev, Alexander N.; New Journal of Chemistry 48 (2024) 1952–1957; doi:10.1039/D3NJ05142K

data_7062929
_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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0171P)^2^+0.2347P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_res_checksum              56229
_shelx_hkl_checksum              11462