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_4111196
_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            'C51 H80 Pr2'
_chemical_formula_weight         974.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                100.103(3)
_cell_angle_beta                 103.126(3)
_cell_angle_gamma                92.613(3)
_cell_formula_units_Z            4
_cell_length_a                   16.585(3)
_cell_length_b                   16.933(3)
_cell_length_c                   17.790(3)
_cell_measurement_temperature    168(2)
_cell_volume                     4771.0(15)
_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      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40897
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.049
_exptl_absorpt_correction_T_max  0.9045
_exptl_absorpt_correction_T_min  0.5601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         16241
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0296P)^2^+20.3341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                10364
_reflns_number_total             16241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0645988si20060706_023754_2.cif
_cod_data_source_block           tmc34
_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_original_cell_volume        4771.1(15)
_cod_database_code               4111196