"Ionic Carbenes": Synthesis, Structural Characterization, and Reactivity of Rare-Earth Metal Methylidene Complexes
H. Martin Dietrich; Karl W. Törnroos; Reiner Anwander; Journal of the American Chemical Society 128 (2006) 9298–9299; doi:10.1021/ja062523y

data_4110729
_publ_contact_author_address
;
Department of Chemistry
University of Bergen
All\'egaten 41
N-5007 Bergen
Norway
;
_publ_contact_author_name        'Reiner Anwander'
_publ_section_title
;
 "Ionic Carbenes": Synthesis, Structural Characterization, and Reactivity
 of Rare-Earth Metal Methylidene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9298
_journal_page_last               9299
_journal_paper_doi               10.1021/ja062523y
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C43 H71 Cl4 O3 Y3'
_chemical_formula_sum            'C43 H71 Cl4 O3 Y3'
_chemical_formula_weight         1044.53
_chemical_name_common
;
[Cp^*^~3~Y~3~(\m-Cl)3(\m3-Cl)(\m3-CH~2~)(THF)~3]
;
_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                 91.1070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5935(6)
_cell_length_b                   19.8342(9)
_cell_length_c                   18.6469(9)
_cell_measurement_reflns_used    19762
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.185
_cell_volume                     4656.8(4)
_computing_cell_refinement
;
Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.059, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_molecular_graphics
;
Brandenburg, K. (2005). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, 
Germany.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of 
G\"ottingen, Germany.
;
_computing_structure_solution
;     
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of 
G\"ottingen, Germany. 
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean '48 \um'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-AXS SMART 2K CCD'
_diffrn_measurement_method       '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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78281
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  '32 h'
_diffrn_standards_number         1142
_exptl_absorpt_coefficient_mu    3.973
_exptl_absorpt_correction_T_max  0.54211
_exptl_absorpt_correction_T_min  0.26163
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Bruker AXS (2003). SHELXTL. Version 6.14. 
Bruker AXS Inc., Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       'flat prism'
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.599
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         13582
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0359P)^2^+4.3188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                10911
_reflns_number_total             13582
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja062523ysi20060412_042114.cif
_cod_data_source_block           compound4a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110729