Oxoneptunium(V) as part of the framework of a polyoxometalate
Copping, Roy; Gaunt, Andrew J.; May, Iain; Sharrad, Clint A.; Collison, David; Helliwell, Madeleine; Fox, O. Danny; Jones, Chris J.; Chemical Communications (Cambridge, United Kingdom)  (2006) 3788–3790; doi:10.1039/b608589j

data_7101393
_publ_section_title
;
 Oxoneptunium(V) as part of the framework of a polyoxometalate
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   36
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3788
_journal_page_last               3790
_journal_paper_doi               10.1039/b608589j
_journal_year                    2006
_chemical_formula_sum            'Bi3 H180 N14 Na4 Np3 O179 W30.72'
_chemical_formula_weight         10319.35
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.600(5)
_cell_angle_beta                 81.457(5)
_cell_angle_gamma                62.067(5)
_cell_formula_units_Z            2
_cell_length_a                   18.580(5)
_cell_length_b                   18.767(5)
_cell_length_c                   24.137(5)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.60
_cell_measurement_theta_min      2.19
_cell_volume                     7274(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1286
_diffrn_reflns_av_sigmaI/netI    0.2964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38318
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    30.294
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9152
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.967
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.548
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         20745
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2526
_reflns_number_gt                8127
_reflns_number_total             20745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608589j.txt
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'H180 Bi3 N14 Na4 Np3 O179 W30.72'
_cod_database_code               7101393