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_4342674
_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            'C77 H110 I N2 O Si Sm2'
_chemical_formula_weight         1535.36
_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                66.042(6)
_cell_angle_beta                 68.459(5)
_cell_angle_gamma                61.546(6)
_cell_formula_units_Z            2
_cell_length_a                   15.4990(8)
_cell_length_b                   16.0862(10)
_cell_length_c                   19.1763(10)
_cell_measurement_reflns_used    7586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.0760
_cell_measurement_theta_min      3.2380
_cell_volume                     3750.5(4)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27377
_diffrn_reflns_theta_full        73.78
_diffrn_reflns_theta_max         73.7821
_diffrn_reflns_theta_min         3.2576
_exptl_absorpt_coefficient_mu    15.321
_exptl_absorpt_correction_T_max  0.6564
_exptl_absorpt_correction_T_min  0.2407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.787
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         14637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                10721
_reflns_number_total             14637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502991p_si_001.cif
_cod_data_source_block           7_cu-496-p1
_cod_depositor_comments
'Adding full bibliography for 4342667--4342674.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4342674