Open-Shell Lanthanide(II+) or -(III+) Complexes Bearing σ-Silyl and Silylene Ligands: Synthesis, Structure, and Bonding Analysis.
Zitz, Rainer; Arp, Henning; Hlina, Johann; Walewska, Małgorzata; Marschner, Christoph; Szilvási, Tibor; Blom, Burgert; Baumgartner, Judith; Inorganic chemistry 54 (2015) 3306–3315; doi:10.1021/ic502991p

data_4342672
_publ_section_title
;
 Open-Shell Lanthanide(II+) or -(III+) Complexes Bearing \s-Silyl and
 Silylene Ligands: Synthesis, Structure, and Bonding Analysis.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3306
_journal_page_last               3315
_journal_paper_doi               10.1021/ic502991p
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C39 H62 N2 O Si Sm'
_chemical_formula_weight         753.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.5232(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.24887(19)
_cell_length_b                   16.5538(2)
_cell_length_c                   16.6349(2)
_cell_measurement_reflns_used    8629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4820
_cell_measurement_theta_min      3.9880
_cell_volume                     3919.92(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2717
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16047
_diffrn_reflns_theta_full        73.66
_diffrn_reflns_theta_max         73.6614
_diffrn_reflns_theta_min         3.1044
_exptl_absorpt_coefficient_mu    11.752
_exptl_absorpt_correction_T_max  0.5911
_exptl_absorpt_correction_T_min  0.1648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.813
_refine_diff_density_min         -1.954
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1003P)^2^+4.3391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                6712
_reflns_number_total             7695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502991p_si_001.cif
_cod_data_source_block           5_cu-476
_cod_depositor_comments
'Adding full bibliography for 4342667--4342674.cif.'
_cod_original_cell_volume        3919.91(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4342672