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_4338283
_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_formula_moiety         '5(C16 H36 N), 4(C2 H3 N), O62 S2 V W17'
_chemical_formula_sum            'C88 H192 N9 O62 S2 V W17'
_chemical_formula_weight         5609.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.853(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   26.1401(5)
_cell_length_b                   15.5551(3)
_cell_length_c                   35.844(3)
_cell_measurement_reflns_used    78150
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.25
_cell_volume                     14020.3(14)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0458
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            91799
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.075
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             10368.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.520
_refine_diff_density_min         -2.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     810
_refine_ls_number_reflns         15998
_refine_ls_number_restraints     979
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0233P)^2^+229.8953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                13525
_reflns_number_total             15998
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic402994q_si_002.cif
_cod_data_source_block           No.4
_cod_depositor_comments
'Adding full bibliography for 4338282--4338283.cif.'
_cod_original_cell_volume        14020.5(12)
_cod_database_code               4338283