Synthesis and Characterization of Novel Wells-Dawson-Type Mono Vanadium(V)-Substituted Tungsto-polyoxometalate Isomers: 1- and 4-[S2VW17O62](5-).
Ueda, Tadaharu; Ohnishi, Miho; Shiro, Motoo; Nambu, Jun-Ichi; Yonemura, Toshiaki; Boas, John F.; Bond, Alan M.; Inorganic chemistry 53 (2014) 4891–4898; doi:10.1021/ic402994q

data_4338282
_publ_section_title
;
 Synthesis and Characterization of Novel Wells-Dawson-Type Mono
 Vanadium(V)-Substituted Tungsto-polyoxometalate Isomers: 1- and
 4-[S2VW17O62](5-).
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4891
_journal_page_last               4898
_journal_paper_doi               10.1021/ic402994q
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         '5(C12 H28 N), C2 H3 N, O62 S2 V W17'
_chemical_formula_sum            'C62 H143 N6 O62 S2 V W17'
_chemical_formula_weight         5205.33
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.3309(4)
_cell_length_b                   20.3938(4)
_cell_length_c                   30.927(3)
_cell_measurement_reflns_used    194319
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.02
_cell_volume                     11561.6(12)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2000-2010)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku, 2000-2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku VariMax with RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            202709
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.056
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9464.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.840
_refine_diff_density_min         -0.910
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  12210 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1363
_refine_ls_number_reflns         26429
_refine_ls_number_restraints     1676
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0051P)^2^+43.1544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0400
_reflns_number_gt                26023
_reflns_number_total             26429
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic402994q_si_003.cif
_cod_data_source_block           N0.2
_cod_depositor_comments
'Adding full bibliography for 4338282--4338283.cif.'
_cod_original_cell_volume        11561.5(9)
_cod_database_code               4338282