Synthesis and characterization of a new Keggin anion: [BeW12O40]^6-^
Alexander V. Anyushin; Anton I. Smolentsev; Dmitry A. Mainichev; Cristian Vicent; Artem L. Gushchin; Maxim N. Sokolov; Vladimir P. Fedin; Chem.Commun. 50 (2014) 9083–; doi:10.1039/C4cc02456G

data_7115428
_publ_section_title
;
 Synthesis and characterization of a new Keggin anion: [BeW12O40]^6-^
;
_journal_name_full               Chem.Commun.
_journal_page_first              9083
_journal_paper_doi               10.1039/C4cc02456G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'Be O40 W12, 6(C2 H8 N), 4(H2 O)'
_chemical_formula_sum            'C12 H56 Be N6 O44 W12'
_chemical_formula_weight         3203.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.2180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1943(3)
_cell_length_b                   19.4817(5)
_cell_length_c                   21.0895(5)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.64
_cell_measurement_theta_min      2.32
_cell_volume                     5230.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33930
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.69
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.376
_exptl_absorpt_correction_T_max  0.3522
_exptl_absorpt_correction_T_min  0.1779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5656
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.038
_refine_diff_density_min         -2.603
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         11991
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0057P)^2^+289.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                10035
_reflns_number_total             11991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02456g2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7115428