Steric Effects in Lanthanide Sandwich Complexes Containing Bulky Cyclooctatetraenyl Ligands
Edelmann, Anja; Lorenz, Volker; Hrib, Cristian G.; Hilfert, Liane; Blaurock, Steffen; Edelmann, Frank T.; Organometallics 32 (2013) 1435–; doi:10.1021/om3010993

data_4080350
_publ_section_title
;
 Steric Effects in Lanthanide Sandwich Complexes Containing Bulky
 Cyclooctatetraenyl Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1435
_journal_paper_doi               10.1021/om3010993
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C50 H80 Cl2 Nd2 O2 Si4'
_chemical_formula_weight         1184.88
_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                 102.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.462(3)
_cell_length_b                   10.798(2)
_cell_length_c                   21.049(4)
_cell_measurement_reflns_used    674
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      1.98
_cell_volume                     2770.0(10)
_computing_cell_refinement       'Stoe XAREA'
_computing_data_collection       'Stoe XAREA'
_computing_data_reduction        'Stoe XAREA'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       omega-scans
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7450
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.3339
_exptl_absorpt_correction_T_min  0.3176
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
; 
 Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification. 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.217
_refine_diff_density_min         -2.327
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                5794
_reflns_number_total             7450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010993_si_003.cif
_cod_data_source_block           ip2_234a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4080350