Synthesis, Molecular, and Electronic Structure of (η8-C8H8)Ln(scorpionate) Half-Sandwich Complexes: An Experimental Key to a Better Understanding of f-Element-Cyclooctatetraenyl Bonding
Hanns-Dieter Amberger; Frank T. Edelmann; Jochen Gottfriedsen; Regine Herbst-Irmer; Stefan Jank; Ulrike Kilimann; Mathias Noltemeyer; Hauke Reddmann; Martina Schäfer; Inorganic Chemistry 48 (2009) 760–772; doi:10.1021/ic801765n

data_4301234
_publ_contact_author_address
;Institute of Inorganic Chemistry
University of G\"ottingen
Tammannstr. 4
D-37077 G\"ottingen
Germany
;
_publ_contact_author_email       rherbst@shelx.uni-ac.gwdg.de
_publ_contact_author_fax         +49-551-392582
_publ_contact_author_name        'Regine Herbst-Irmer'
_publ_contact_author_phone       +49-551-393007
_publ_section_title
;
Synthesis, Molecular, and Electronic Structure of (\h8-C8H8)Ln(scorpionate)
Half-Sandwich Complexes: An Experimental Key to a Better Understanding of
f-Element-Cyclooctatetraenyl Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              760
_journal_page_last               772
_journal_paper_doi               10.1021/ic801765n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C17 H18 B N6 Sm'
_chemical_formula_weight         467.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-09-15 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4220(10)
_cell_length_b                   13.2330(10)
_cell_length_c                   18.830(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1849.4(4)
_computing_cell_refinement       'Stoe DIF4 Ver.7.08'
_computing_data_collection       'Stoe DIF4 Ver.7.08'
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Stoe-Siemens-AED four circle-diffractometer'
_diffrn_measurement_method       'profile from 2theta/omega'
_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  0.0914
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2089
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         3.59
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.186
_exptl_absorpt_correction_T_max  0.2988
_exptl_absorpt_correction_T_min  0.2508
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.480
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       0.0066(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         1803
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+0.1219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                1765
_reflns_number_total             1803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801765n_si_002_1.cif
_cod_data_source_block           test
_cod_database_code               4301234