Lanthanide(III) and Actinide(III) Complexes [M(BH4)2(THF)5][BPh4] and [M(BH4)2(18-crown-6)][BPh4] (M = Nd, Ce, U): Synthesis, Crystal Structure, and Density Functional Theory Investigation of the Covalent Contribution to Metal-Borohydride Bonding
Thérèse Arliguie; Lotfi Belkhiri; Salah-Eddine Bouaoud; Pierre Thuéry; Claude Villiers; Abdou Boucekkine; Michel Ephritikhine; Inorganic Chemistry 48 (2009) 221–230; doi:10.1021/ic801685v

data_4301117
_publ_section_title
;
Lanthanide(III) and Actinide(III) Complexes [M(BH4)2(THF)5][BPh4] and
[M(BH4)2(18-crown-6)][BPh4] (M = Nd, Ce, U): Synthesis, Crystal Structure,
and Density Functional Theory Investigation of the Covalent Contribution to
Metal-Borohydride Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              221
_journal_page_last               230
_journal_paper_doi               10.1021/ic801685v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C48 H76 B3 Ce O5 S'
_chemical_formula_weight         937.70
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.434(2)
_cell_angle_beta                 101.694(3)
_cell_angle_gamma                100.072(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4292(3)
_cell_length_b                   14.9752(3)
_cell_length_c                   15.4239(4)
_cell_measurement_reflns_used    75230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.93
_cell_volume                     2399.52(12)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and three \w scans with 2\% steps'
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75230
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0950P)^2^+12.5278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                8644
_reflns_number_total             9058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801685v_si_002_2.cif
_cod_data_source_block           3.C~4~H~8~S
_cod_database_code               4301117