Unexpected Tandem Reactions of Tris(cyclopentadieny1)lanthanide with Diphenylketene and Regeneration of the η5-Bonding Mode: One-Pot Synthesis of Heteroleptic Yttrocenes from Simple (C5H5)3Y Precursors
Li, Xiaoqing; Liu, Ruiting; Zhang, Zhengxing; Mu, Xiaoming; Weng, Linhong; Zhou, Xigeng; Organometallics 29 (2010) 3298–; doi:10.1021/om1002045

data_4065940
_publ_section_title
;
 Unexpected Tandem Reactions of Tris(cyclopentadieny1)lanthanide with
 Diphenylketene and Regeneration of the \h5-Bonding Mode: One-Pot
 Synthesis of Heteroleptic Yttrocenes from Simple (C5H5)3Y Precursors
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3298
_journal_paper_doi               10.1021/om1002045
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C93.5 H78 Li O5 Y3'
_chemical_formula_weight         1555.23
_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           SHELXL-97
_cell_angle_alpha                84.452(7)
_cell_angle_beta                 73.025(7)
_cell_angle_gamma                80.230(6)
_cell_formula_units_Z            2
_cell_length_a                   13.253(6)
_cell_length_b                   14.096(6)
_cell_length_c                   21.175(10)
_cell_measurement_reflns_used    857
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.587
_cell_measurement_theta_min      2.397
_cell_volume                     3724(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.2446
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15355
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  0.8906
_exptl_absorpt_correction_T_min  0.7173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.735
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         12825
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.736
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                5110
_reflns_number_total             12825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002045_si_001.cif
_cod_data_source_block           f80705b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C93.50 H78 Li O5 Y3'
_cod_database_code               4065940