The First Structural and Spectroscopic Characterization of a Neptunyl Polyoxometalate Complex
Andrew J. Gaunt; Iain May; Madeleine Helliwell; Steve Richardson; Journal of the American Chemical Society 124 (2002) 13350–13351; doi:10.1021/ja028005e

data_4115288
_publ_section_title
;
 The First Structural and Spectroscopic Characterization of a Neptunyl
 Polyoxometalate Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13350
_journal_page_last               13351
_journal_paper_doi               10.1021/ja028005e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'H39 Na12 Np2 O110 P2 W18'
_chemical_formula_weight         5920.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.7610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.6123(10)
_cell_length_b                   14.4990(9)
_cell_length_c                   21.2765(13)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.279
_cell_measurement_theta_min      2.406
_cell_volume                     4759.5(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'XSHELL, Bruker'
_computing_publication_material  'Diamond 2.1, Crystal Impact'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SMART platform CCD, Bruker'
_diffrn_measurement_method       '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  0.1946
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33582
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    24.037
_exptl_absorpt_correction_T_max  0.7951
_exptl_absorpt_correction_T_min  0.0862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.131
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             5198
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.733
_refine_diff_density_min         -3.032
_refine_diff_density_rms         0.667
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                6151
_reflns_number_total             8369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028005e_s1.cif
_cod_data_source_block           ajg26abs
_cod_database_code               4115288