Insertion of Ketenimines into the Ln−C σ-Bond of Organolanthanides: A New Strategy for Synthesis of Lanthanide 1-Azaallyl Complexes
Zhang, Zhengxing; Bu, Xiuli; Zhang, Jie; Liu, Ruiting; Zhou, Xigeng; Weng, Linhong; Organometallics 29 (2010) 2111–; doi:10.1021/om100089a

data_4065700
_publ_section_title
;
 Insertion of Ketenimines into the Ln&#x2212;C \s-Bond of
 Organolanthanides: A New Strategy for Synthesis of Lanthanide 1-Azaallyl
 Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2111
_journal_paper_doi               10.1021/om100089a
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C29 H32 N Y'
_chemical_formula_weight         483.47
_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                 112.204(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.750(11)
_cell_length_b                   10.820(6)
_cell_length_c                   23.573(12)
_cell_measurement_reflns_used    967
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.362
_cell_measurement_theta_min      2.507
_cell_volume                     4900(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1115
_diffrn_reflns_av_sigmaI/netI    0.1876
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19481
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  0.7620
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1638
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                3382
_reflns_number_total             8618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100089a_si_002.cif
_cod_data_source_block           1-Y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4900(4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065700