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_7101394
_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            'H278 N29 Na7 Np6 O315 Sb6 W61.06'
_chemical_formula_weight         19264.97
_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                69.3050(10)
_cell_angle_beta                 80.4880(10)
_cell_angle_gamma                66.4160(10)
_cell_formula_units_Z            2
_cell_length_a                   22.3826(13)
_cell_length_b                   27.3954(16)
_cell_length_c                   30.0087(17)
_cell_measurement_reflns_used    5969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.27
_cell_volume                     15769.6(16)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1173
_diffrn_reflns_av_sigmaI/netI    0.2345
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            97487
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    24.735
_exptl_absorpt_correction_T_max  0.6375
_exptl_absorpt_correction_T_min  0.2763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             16912
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.497
_refine_diff_density_min         -5.876
_refine_diff_density_rms         0.459
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         45111
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                19213
_reflns_number_total             45111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608589j.txt
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7101394