Crystal structures of two decavanadates(V) with pentaaquamanganese(II) pendant groups: (NMe~4~)~2~[V~10~O~28~{Mn(H~2~O)~5~}~2~]·5H~2~O and [NH~3~C(CH~2~OH)~3~]~2~[V~10~O~28~{Mn(H~2~O)~5~}~2~]·2H~2~O
Franco, Maurício P.; Rüdiger, André Luis; Soares, Jaísa F.; Nunes, Giovana G.; Hughes, David L.; Acta Crystallographica Section E 71 (2015) 146–150; doi:10.1107/S2056989014028230

data_2240372
_publ_section_title
;
 Crystal structures of two decavanadates(V) with pentaaquamanganese(II)
 pendant groups: (NMe~4~)~2~[V~10~O~28~{Mn(H~2~O)~5~}~2~]&#x00B7;5H~2~O
 and [NH~3~C(CH~2~OH)~3~]~2~[V~10~O~28~{Mn(H~2~O)~5~}~2~]&#x00B7;2H~2~O
;
_journal_coeditor_code           HB7337
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              146
_journal_page_last               150
_journal_paper_doi               10.1107/S2056989014028230
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C4 H12 N O3)2 [Mn2 V10 O28 (H2 O1)10], 2H2 O'
_chemical_formula_moiety         '2(C4 H12 N O3 +), V10 O38 H20 Mn2 2-, 2(H2 O)'
_chemical_formula_structural
'[NH3C(CH2OH)3]2, [V10 O28 {Mn(H2O)5}2], 2(H2O)'
_chemical_formula_sum            'C8 H48 Mn2 N2 O46 V10'
_chemical_formula_weight         1527.76
_chemical_name_systematic
;Bis{[tris(hydroxymethyl)methyl]ammonium}
decaaquadi-\m~4~oxido-tetra-\m~3~-oxido-hexadeca-\m~2~-oxido-hexaoxidodimanganesedecavanadate dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.3920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3147(8)
_cell_length_b                   9.7733(4)
_cell_length_c                   22.7952(10)
_cell_measurement_reflns_used    38099
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      3.02
_cell_volume                     4276.3(3)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71752
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.449
_diffrn_reflns_theta_min         2.877
_exptl_absorpt_coefficient_mu    2.778
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0062P)^2^+110.7865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                3280
_reflns_number_total             3936
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7337sup1.cif
_cod_data_source_block           Compound-B
_cod_database_code               2240372
_shelx_estimated_absorpt_t_min   0.343
_shelx_estimated_absorpt_t_max   0.714
_shelx_hkl_checksum              29000
_shelx_res_checksum              42660