Polyoxoanions assembled by the condensation of vanadate, tungstate and selenite: solution studies and crystal structures of the mixed metal derivatives (NMe4)2Na2[WVI4VV2O19]·8H2O and (NMe4)4.83[(SeIVWVI4.57VV4.43O33)2(WVI(O)(H2O))(VVO)2.6]·10.57H2O
Abramov, Pavel A.; Peresypkina, Eugenia V.; Izarova, Natalia V.; Vicent, Cristian; Zhdanov, Artem A.; Kompankov, Nikolay B.; Gutsul, Tatiana; Sokolov, Maxim N.; New J. Chem. 40 (2016) 937–; doi:10.1039/C5NJ00858A

data_7054917
_publ_section_title
;
 Polyoxoanions assembled by the condensation of vanadate, tungstate and
 selenite: solution studies and crystal structures of the mixed metal
 derivatives (NMe4)2Na2[WVI4VV2O19]&#x00B7;8H2O and
 (NMe4)4.83[(SeIVWVI4.57VV4.43O33)2(WVI(O)(H2O))(VVO)2.6]&#x00B7;10.57H2O
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_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              937
_journal_paper_doi               10.1039/C5NJ00858A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_structural     '(N Me4)2 Na2[(W4 V2) O19] * 8(H2 O)'
_chemical_formula_sum            'C8 H40 N2 Na2 O27 V2 W4'
_chemical_formula_weight         1479.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-07 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6008(10)
_cell_length_b                   9.9127(5)
_cell_length_c                   18.2252(9)
_cell_measurement_reflns_used    6863
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      30.3334
_cell_measurement_theta_min      2.4586
_cell_volume                     3360.4(3)
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker DUO CCD detector'
_diffrn_measurement_method       'combined omega- and phi-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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23362
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.292
_exptl_absorpt_correction_T_max  0.0998
_exptl_absorpt_correction_T_min  0.0532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.925
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.138
_refine_diff_density_max         2.870
_refine_diff_density_min         -2.557
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0133P)^2^+87.8184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                3682
_reflns_number_total             4082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00858a2.cif
_cod_data_source_block           sof
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7054917--7054918.cif.
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_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7054917