Structure Determination of Neptunium(VI) μ3-Hydroxobenzoate, [(NpO2)2(μ3-OH)2(H5C6COO)2].2H2O
Iraida A. Charushnikova; Nikolai N. Krot; Vadim I. Makarenkov; Inorganic Chemistry 49 (2010) 7611–7613; doi:10.1021/ic100951y

data_4316406
_publ_section_title
;
 Structure Determination of Neptunium(VI) \m3-Hydroxobenzoate,
 [(NpO2)2(\m3-OH)2(H5C6COO)2].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7611
_journal_page_last               7613
_journal_paper_doi               10.1021/ic100951y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C14 H12 Np2 O10, 2(O H2)'
_chemical_formula_sum            'C14 H16 Np2 O12'
_chemical_formula_weight         850.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   38.4784(10)
_cell_length_b                   38.4784(10)
_cell_length_c                   8.7086(2)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      3.82
_cell_volume                     11166.4(5)
_computing_cell_refinement       SAINT-Plus
_computing_data_collection       SMART
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHRLXTL97
_computing_publication_material  SHELXTL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD area detector'
_diffrn_measurement_method       '\f- and \w-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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35033
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    8.376
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6876
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.788
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0696P)^2^+523.7540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                4103
_reflns_number_total             4962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100951y_si_002.cif
_cod_data_source_block           npbb
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4316406