Dihydrogen Addition in a Dinuclear Rare-Earth Metal Hydride Complex Supported by a Metalated TREN Ligand
Ajay Venugopal; Waldemar Fegler; Thomas P. Spaniol; Laurent Maron; Jun Okuda; Journal of the American Chemical Society 133 (2011) 17574–17577; doi:10.1021/ja207180x

data_4107057
_publ_contact_author
;       Jun Okuda
        Institute of Inorganic Chemistry
        RWTH Aachen University
        Landoltweg 1
        D-52056 Aachen
        Germany
;
_publ_contact_author_email       jun.okuda@ac.rwth-aachen.de
_publ_contact_author_fax         '+49 241 80 92644'
_publ_contact_author_phone       '+49 241 80 94645'
_publ_section_title
;
 Dihydrogen Addition in a Dinuclear Rare-Earth Metal Hydride Complex
 Supported by a Metalated TREN Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17574
_journal_page_last               17577
_journal_paper_doi               10.1021/ja207180x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C24 H62 N8 Y2, 2(C32 H12 B F24), 2 (C4 H10 O)'
_chemical_formula_sum            'C96 H106 B2 F48 N8 O2 Y2'
_chemical_formula_weight         2515.33
_chemical_name_systematic
;
 ?
;
_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                69.3026(13)
_cell_angle_beta                 70.1548(14)
_cell_angle_gamma                80.9762(14)
_cell_formula_units_Z            1
_cell_length_a                   12.8104(11)
_cell_length_b                   13.9351(12)
_cell_length_c                   17.2719(14)
_cell_measurement_reflns_used    4665
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      1.3
_cell_volume                     2710.6(4)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'APEX Area Detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'INCOATEC microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32822
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7701
_exptl_absorpt_correction_T_min  0.7226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Mulabs'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       block
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                6924
_reflns_number_total             11195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207180x_si_002_5.cif
_cod_data_source_block           4-Y
_cod_database_code               4107057