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_4112951
_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 V W12'
_chemical_formula_weight         3866.97
_chemical_name_systematic
; 
 ? 
;
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
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_cell_length_b                   17.588(3)
_cell_length_c                   17.588(3)
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_computing_cell_refinement       'SMART, Bruker (2000)'
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_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16645
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    12.778
_exptl_absorpt_correction_T_max  0.1142
_exptl_absorpt_correction_T_min  0.0799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_description       block
_exptl_crystal_F_000             3574
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.958
_refine_diff_density_min         -3.696
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1227
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+19.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                1081
_reflns_number_total             1227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0475499si20040502_022036.cif
_cod_data_source_block           tatp002
_cod_original_cell_volume        5440.7(13)
_cod_database_code               4112951