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_7054918
_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
;
_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)4.83 [(Se W4.57 V4.43 O33)2 (W O (H2O)) (V O)2.6] * 10.57(H2 O)'
_chemical_formula_sum            'C19.32 H81.1 N4.83 O81.17 Se2 V11.46 W10.14'
_chemical_formula_weight         4286.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-10-10 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.4257(11)
_cell_length_b                   21.2136(11)
_cell_length_c                   12.9194(6)
_cell_measurement_reflns_used    8210
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.10
_cell_measurement_theta_min      4.00
_cell_volume                     5323.9(5)
_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_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker DUO CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39238
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.831
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    29.320
_exptl_absorpt_correction_T_max  0.3197
_exptl_absorpt_correction_T_min  0.1438
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_description       block
_exptl_crystal_F_000             3924
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.171
_refine_diff_density_min         -2.586
_refine_diff_density_rms         0.223
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         8396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+29.2398P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                6877
_reflns_number_total             8396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00858a2.cif
_cod_data_source_block           14
_cod_depositor_comments
;Adding full bibliography for 7054917--7054918.cif.

The following automatic conversions were performed:
'_symmetry_space_group_it_number' data item was removed -- it should
have been renamed to '_space_group_IT_number' as specified in the
replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_it_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_formula_sum
'C19.32 H81.10 N4.83 O81.17 Se2 V11.46 W10.14'
_cod_database_code               7054918
_shelxl_version_number           2013-2
_shelx_res_checksum              51701