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_4301235
_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            'C27 H38 B Ce N6 O'
_chemical_formula_weight         613.56
_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     heavy
_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                 103.020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0860(10)
_cell_length_b                   21.317(2)
_cell_length_c                   15.906(2)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2671.2(5)
_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-92
_computing_structure_refinement  SHELXL-92
_computing_structure_solution    SHELXS-92
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device
'Stoe-Siemens-Huber-AED2 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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3730
_diffrn_reflns_theta_full        22.60
_diffrn_reflns_theta_max         22.60
_diffrn_reflns_theta_min         4.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_T_max  0.5818
_exptl_absorpt_correction_T_min  0.4486
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     982
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0348P)^2^+3.8520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                2913
_reflns_number_total             3509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801765n_si_002_2.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301235