51V Magic Angle Spinning NMR Spectroscopy of Six-Coordinate Lindqvist Oxoanions: A Sensitive Probe for the Electronic Environment in Vanadium-Containing Polyoxometalates. Counterions Dictate the 51V Fine Structure Constants in Polyoxometalate Solids
Wenlin Huang; Louis Todaro; Lynn C. Francesconi; Tatyana Polenova; Journal of the American Chemical Society 125 (2003) 5928–5938; doi:10.1021/ja029246p

data_4113724
_publ_contact_author_address
;
Department of Chemistry
City University of New York- Hunter College
695 Park Avenue
New York, NY 10021
United States of America
;
_publ_contact_author_email       tpolenov@hunter.cuny.edu
_publ_contact_author_name        'Dr. Tatyana Polenova'
_publ_section_title
;
 51V Magic Angle Spinning NMR Spectroscopy of Six-Coordinate Lindqvist
 Oxoanions: A Sensitive Probe for the Electronic Environment in
 Vanadium-Containing Polyoxometalates. Counterions Dictate the 51V Fine
 Structure Constants in Polyoxometalate Solids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5928
_journal_page_last               5938
_journal_paper_doi               10.1021/ja029246p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C48 H108 N3 O19 V2 W4'
_chemical_formula_weight         1868.637
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           manual
_cell_angle_alpha                90
_cell_angle_beta                 112.40(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.135(7)
_cell_length_b                   18.377(2)
_cell_length_c                   27.279(4)
_cell_measurement_reflns_used    6356
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2.161
_cell_volume                     13967(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_number            6356
_diffrn_reflns_theta_max         60
_diffrn_reflns_theta_min         2.161
_exptl_absorpt_coefficient_mu    165.74
_exptl_absorpt_correction_T_max  23.07
_exptl_absorpt_correction_T_min  1.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    not_measured
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.47
_refine_diff_density_min         -1.44
_refine_ls_extinction_method     none
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+1.0418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.072
_reflns_number_gt                6356
_reflns_number_total             10364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029246psi20030204_050641.cif
_cod_data_source_block           2vbhz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        13966.9(46)
_cod_original_formula_sum        'C48 H108 N3 V2 W4 O19'
_cod_database_code               4113724