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_1514781
_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
'2(C24 H24 F9 N9 O9 P S4 Sm), C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C54 H61 F18 N19 O19 P2 S8 Sm2'
_chemical_formula_weight         2241.44
_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                 97.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.764(2)
_cell_length_b                   19.857(4)
_cell_length_c                   22.899(5)
_cell_measurement_reflns_used    29512
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      3.90
_cell_volume                     4403.1(16)
_computing_cell_refinement       'CrysAlis Red'
_computing_data_collection       'CrysAlis CCD'
_computing_data_reduction        'CrysAlis Red'
_computing_molecular_graphics    Ortep32
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe Stadi with CCD'
_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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29512
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                4973
_reflns_number_total             7495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc50708d.txt
_cod_data_source_block           compound_[Sm(1)(Otf)3]
_cod_original_cell_volume        4403.2(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1514781