Chemoprotective activity of mixed valence polyoxovanadates against diethylsulfate in E. coli cultures: insights from chemichal speciation studies
Postal, Kahoana; Maluf, Daniela Florêncio; Valdameri, Glaucio; Rüdiger, André Luis; Hughes, David L.; Sa, Eduardo Lemos de; Ribeiro, Ronny R.; Souza, Emanuel Maltempi de; Fernandes Soares, Jaisa; Nunes, Giovana G.; RSC Adv.  (2016) –; doi:10.1039/C6RA15826A

data_7227230
_publ_section_title
;
 Chemoprotective activity of mixed valence polyoxovanadates against
 diethylsulfate in E. coli cultures: insights from chemichal speciation
 studies
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA15826A
_journal_year                    2016
_chemical_formula_moiety         '0.5K, 3.5(N H4), H6 O42 P V14, 12(H2 O)'
_chemical_formula_structural     '0.5K, 3.5(NH4), {H6O38V14(PO4)}, 12(H2O)'
_chemical_formula_sum            'H44 K0.5 N3.5 O54 P V14'
_chemical_formula_weight         1721.06
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7844(5)
_cell_length_b                   24.2257(11)
_cell_length_c                   16.3820(7)
_cell_measurement_reflns_used    34692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      3.08
_cell_volume                     4585.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material
'SHELXL-2014 (Sheldrick, 2015) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_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  0.0477
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61802
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_min         3.527
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.930
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             3388
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+9.6061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra15826a2.cif
_cod_data_source_block           kp198-3
_cod_original_formula_sum        'H44 K0.50 N3.50 O54 P V14'
_cod_database_code               7227230
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              71181