A series of inorganic aggregates composed of [MnV13O38]7− polyoxoanions and transition metal cations
Lan, Qing; Tan, Huaqiao; Liu, Ding; Wang, Enbo; Journal of Solid State Chemistry 199 (2013) 129–133; doi:10.1016/j.jssc.2012.12.005

data_1562713
_publ_section_title
;
 A series of inorganic aggregates composed of [MnV13O38]7&#x2212;
 polyoxoanions and transition metal cations
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              129
_journal_page_last               133
_journal_paper_doi               10.1016/j.jssc.2012.12.005
_journal_volume                  199
_journal_year                    2013
_chemical_formula_sum            'H44 K0.5 Mn Na2.5 Ni2 O60 V13'
_chemical_formula_weight         1915.96
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.45(3)
_cell_angle_beta                 81.65(3)
_cell_angle_gamma                62.78(3)
_cell_formula_units_Z            2
_cell_length_a                   11.871(2)
_cell_length_b                   11.972(2)
_cell_length_c                   20.475(4)
_cell_measurement_reflns_used    8698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.02
_cell_volume                     2554.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1177
_diffrn_reflns_av_sigmaI/netI    0.1529
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19503
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1882
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.659
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0813
_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/[\s^2^(Fo^2^)+(0.0905P)^2^+12.5842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2398
_reflns_number_gt                4523
_reflns_number_total             8698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-199-129.cif
_cod_data_source_block           3
_cod_original_cell_volume        2554.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H44 K0.50 Mn Na2.50 Ni2 O60 V13'
_cod_database_code               1562713