Lanthanide(III) Sandwich and Half-Sandwich Complexes with Bulky Cyclooctatetraenyl Ligands: Synthesis, Structures, and Magnetic Properties
Volker Lorenz; Phil Liebing; Michael Böhme; Axel Buchholz; Winfried Plass; Niklas Geue; Liane Hilfert; Sabine Busse; Felix Engelhardt; Cristian G. Hrib; Frank T. Edelmann; European Journal of Inorganic Chemistry 2017 (2017) 4840–4849; doi:10.1002/ejic.201700878

data_4039029
_publ_contact_author             'Frank T. Edelmann'
_publ_contact_author_email       frank.edelmann@ovgu.de
_publ_section_title
;
 Lanthanide(III) Sandwich and Half-Sandwich Complexes with Bulky
 Cyclooctatetraenyl Ligands: Synthesis, Structures, and Magnetic
 Properties
;
_journal_coden_ASTM              EJICFO
_journal_issue                   41
_journal_name_full               'European Journal of Inorganic Chemistry'
_journal_page_first              4840
_journal_page_last               4849
_journal_paper_doi               10.1002/ejic.201700878
_journal_volume                  2017
_journal_year                    2017
_chemical_formula_moiety         'C28 H48 Si4 Tb, C12 H30 Li O6'
_chemical_formula_sum            'C40 H78 Li O6 Si4 Tb'
_chemical_formula_weight         933.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                99.284(2)
_cell_angle_beta                 102.123(2)
_cell_angle_gamma                99.692(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4950(3)
_cell_length_b                   12.2906(4)
_cell_length_c                   18.4734(6)
_cell_measurement_reflns_used    24315
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.301
_cell_measurement_theta_min      1.853
_cell_volume                     2462.37(13)
_computing_cell_refinement       'X-Area (STOE & Cie, 2002)'
_computing_data_collection       'X-Area (STOE & Cie, 2002)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 2002)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SIR-97 (Altamore et al., 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21395
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.8668
_exptl_absorpt_correction_T_min  0.7372
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area and X-Red (STOE & Cie, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         4.340
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+3.8485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8196
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            li0182.cif
_cod_data_source_block           li0182
_cod_database_code               4039029
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.846
_shelx_res_checksum              47654
_shelx_hkl_checksum              95506