Exploring the solution behavior of f-element coordination compounds: a case study on some trivalent rare earth and plutonium complexes
Löble, Matthias W.; Oña-Burgos, Pascual; Fernández, Ignacio; Apostolidis, Christos; Morgenstern, Alfred; Walter, Olaf; Bruchertseifer, Frank; Kaden, Peter; Vitova, Tonya; Rothe, Jörg; Dardenne, Kathy; Banik, Nidhu L.; Geist, Andreas; Denecke, Melissa A.; Breher, Frank; Chemical Science 4 (2013) 3717–; doi:10.1039/c3sc50708d

data_1514782
_publ_section_title
;
 Exploring the solution behavior of f-element coordination compounds: a
 case study on some trivalent rare earth and plutonium complexes
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3717
_journal_paper_doi               10.1039/c3sc50708d
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C21 H24 N9 P S, C3 F9 O9 Pu S3, 3(C2 H3 N)'
_chemical_formula_sum            'C30 H33 F9 N12 O9 P Pu S4'
_chemical_formula_weight         1277.89
_chemical_name_systematic
;
1,2-bis(2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)-
3-methyl-2,4,5-trisila-1,3-
distannabicylo[1.1.1]pentan)ethyne
;
_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                83.93
_cell_angle_beta                 70.1560(10)
_cell_angle_gamma                80.1230(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2866(4)
_cell_length_b                   13.3751(5)
_cell_length_c                   13.8490(5)
_cell_measurement_reflns_used    7875
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.55
_cell_volume                     2277.65(14)
_computing_cell_refinement       'APEX II (Bruker 2007)'
_computing_data_collection       'APEX II (Bruker 2007)'
_computing_data_reduction        'SAINT (Bruker 2007)'
_computing_molecular_graphics    'Ortep32 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.715
_diffrn_measured_fraction_theta_max 0.715
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '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  0.0079
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7875
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             1246
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         7093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0250P)^2^+3.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                6834
_reflns_number_total             7093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc50708d.txt
_cod_data_source_block           compound_[Pu(1)(Otf)3]
_cod_original_cell_volume        2277.64(14)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514782