Structural Variability in Neptunium(V) Oxalate Compounds: Synthesis and Structural Characterization of Na2NpO2(C2O4)OH.H2O
Amanda C. Bean; Eduardo Garcia; Brian L. Scott; Wolfgang Runde; Inorganic Chemistry 43 (2004) 6145–6147; doi:10.1021/ic0492082

data_4311653
_publ_contact_author_address
; Nuclear Material Technology
 Los Alamos National Laboratory
 Los Alamos, NM 87545
;
_publ_contact_author_email       bean@lanl.gov
_publ_contact_author_fax         '(505) 665-1780'
_publ_contact_author_name        'Amanda C. Bean'
_publ_contact_author_phone       '(505) 665-1551'
_publ_section_title
;
 Structural Variability in Neptunium(V) Oxalate Compounds: Synthesis and
 Structural Characterization of Na2NpO2(C2O4)OH.H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6145
_journal_page_last               6147
_journal_paper_doi               10.1021/ic0492082
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C2 H3 Na2 Np O8'
_chemical_formula_weight         438.02
_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                 92.997(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.147(5)
_cell_length_b                   18.830(13)
_cell_length_c                   6.688(5)
_cell_measurement_temperature    203(2)
_cell_volume                     773.1(10)
_computing_cell_refinement       'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_data_collection       'Siemens SMART (v. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device_type  'Bruker P4/CCD/PC'
_diffrn_measurement_method       '0.3 degree \f 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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3536
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    13.564
_exptl_absorpt_correction_T_max  0.196
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal-shaped
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.132
_refine_diff_density_min         -3.504
_refine_diff_density_rms         0.385
_refine_ls_extinction_coef       0.0001(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                1057
_reflns_number_total             1333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0492082si20040812_012517.cif
_cod_data_source_block           ccd771
_cod_original_formula_sum        'H3 C2 Na2 Np O8'
_cod_database_code               4311653