High-Yield Synthesis and Single-Crystal X-ray Structure of a Plutonium(III) Aquo Complex: [Pu(H2O)9][CF3SO3]3
John H. Matonic; Brian L. Scott; Mary P. Neu; Inorganic Chemistry 40 (2001) 2638–2639; doi:10.1021/ic015509p

data_4319800
_publ_contact_author
;
     Mary P. Neu
     MS G739
     Los Alamos National Laboratory
     Los Alamos, NM 87545
;
_publ_contact_author_email       mneu@lanl.gov
_publ_contact_author_fax         '505 665 4624'
_publ_contact_author_phone       '505 667 9313'
_publ_section_title
;
 High-Yield Synthesis and Single-Crystal X-ray Structure of a
 Plutonium(III) Aquo Complex: [Pu(H2O)9][CF3SO3]3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2638
_journal_page_last               2639
_journal_paper_doi               10.1021/ic015509p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C3 H18 F9 O18 Pu S3'
_chemical_formula_weight         851.35
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.9283(6)
_cell_length_b                   13.9283(6)
_cell_length_c                   7.3816(4)
_cell_measurement_reflns_used    4192
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      1.69
_cell_volume                     1240.16(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    'Bruker AXS SHEXTL (v. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measurement_device       'Siemens P4/PC'
_diffrn_measurement_method       '\w and \p 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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6672
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_description       needle
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.217
_refine_ls_goodness_of_fit_obs   1.223
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_restrained_S_obs      1.223
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_obs          0.0243
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.5357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0466
_refine_ls_wR_factor_obs         0.0452
_reflns_number_observed          1002
_reflns_number_total             1068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic015509p_s2.cif
_cod_data_source_block           Puaquo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.5357P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.5357P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319800