Planar Trimethylenemethane Dianion Chemistry of Lanthanide Metallocenes: Synthesis, Structure, Density Functional Theory Analysis, and Reactivity of [(C5Me5)2Ln]2[μ-η3:η3-C(CH2)3] Complexes
William J. Evans; Timothy M. Champagne; Joseph W. Ziller; Nikolas Kaltsoyannis; Journal of the American Chemical Society 128 (2006) 16178–16189; doi:10.1021/ja0645988

data_4111199
_publ_section_title
;
 Planar Trimethylenemethane Dianion Chemistry of Lanthanide Metallocenes:
 Synthesis, Structure, Density Functional Theory Analysis, and Reactivity
 of [(C5Me5)2Ln]2[\m-\h3:\h3-C(CH2)3] Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16178
_journal_page_last               16189
_journal_paper_doi               10.1021/ja0645988
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C76 H100 O2 Sm2'
_chemical_formula_weight         1346.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.023(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4167(16)
_cell_length_b                   21.6057(18)
_cell_length_c                   35.253(3)
_cell_measurement_temperature    158(2)
_cell_volume                     13548(2)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            131891
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.7541
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.936
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1447
_refine_ls_number_reflns         27683
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.260
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+86.6507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                20440
_reflns_number_total             27683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0645988si20060706_023754_5.cif
_cod_data_source_block           tmc26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4111199