51V Magic Angle Spinning NMR Spectroscopy of Keggin Anions [PVnW12-nO40](3+n)-: Effect of Countercation and Vanadium Substitution on Fine Structure Constants
Wenlin Huang; Louis Todaro; Glenn P. A. Yap; Robert Beer; Lynn C. Francesconi; Tatyana Polenova; Journal of the American Chemical Society 126 (2004) 11564–11573; doi:10.1021/ja0475499

data_4112949
_publ_section_title
;
 51V Magic Angle Spinning NMR Spectroscopy of Keggin Anions
 [PVnW12-nO40](3+n)-: Effect of Countercation and Vanadium Substitution on
 Fine Structure Constants
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11564
_journal_page_last               11573
_journal_paper_doi               10.1021/ja0475499
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C64 H144 N4 O40 P W12'
_chemical_formula_weight         3847.00
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.6299(7)
_cell_length_b                   18.6299(7)
_cell_length_c                   14.3535(10)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.83
_cell_volume                     4981.7(4)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15371
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    13.883
_exptl_absorpt_correction_T_max  0.1289
_exptl_absorpt_correction_T_min  0.1031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.565
_exptl_crystal_description       block
_exptl_crystal_F_000             3558
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4685(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+64.9228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                5100
_reflns_number_total             5744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0475499si20040502_022002.cif
_cod_data_source_block           tatp001
_cod_database_code               4112949