Synthesis and crystal structure of a ten-coordinate plutonium(iv) ion complexed by 2-[(diphenylphosphino)methyl]pyridine N,P-dioxide: [Pu(NO3)3{2-[(C6H5)2P(O)CH2]C5H4NO}2][Pu(NO3)6]0.5
Matonic, John H.; Neu, Mary P.; Enriquez, Alejandro E.; Paine, Robert T.; Scott, Brian L.; Journal of the Chemical Society, Dalton Transactions  (2002) 2328–; doi:10.1039/b106624m

data_7011015
_publ_section_title
;
 Synthesis and crystal structure of a ten-coordinate plutonium(iv) ion
 complexed by 2-[(diphenylphosphino)methyl]pyridine N,P-dioxide:
 [Pu(NO3)3{2-[(C6H5)2P(O)CH2]C5H4NO}2][Pu(NO3)6]0.5
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2328
_journal_paper_doi               10.1039/b106624m
_journal_year                    2002
_chemical_formula_sum            'C36 H32 N8 O22 P2 Pu1.5'
_chemical_formula_weight         1353.64
_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                65.1950(10)
_cell_angle_beta                 80.5710(10)
_cell_angle_gamma                72.3810(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0407(6)
_cell_length_b                   14.2228(7)
_cell_length_c                   15.6363(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      1.63
_cell_volume                     2314.58(19)
_computing_cell_refinement       'SAINT 4.05  (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05  (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker P4/PC ccd'
_diffrn_measurement_method       '/w and /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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11151
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   'empirical (SADABS, Sheldrick 1996)'
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         6115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0267P)^2^+4.7376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                5439
_reflns_number_total             6115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106624m.txt
_cod_data_source_block           xl
_cod_original_formula_sum        'C36 H32 N8 O22 P2 Pu1.50'
_cod_database_code               7011015