Sandwich Lutetacyclopentadiene with the Coordination of Lithium to the Diene Unit: Synthesis, Structure, and Transformation
Xu, Ling; Wang, Yang; Wang, Yu-Chen; Wang, Zitao; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 35 (2015) 5–; doi:10.1021/acs.organomet.5b00957

data_4088242
_publ_section_title
;
 Sandwich Lutetacyclopentadiene with the Coordination of Lithium to the
 Diene Unit: Synthesis, Structure, and Transformation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              5
_journal_paper_doi               10.1021/acs.organomet.5b00957
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C36 H46 Li Lu O Si2'
_chemical_formula_sum            'C36 H46 Li Lu O Si2'
_chemical_formula_weight         732.82
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.548(3)
_cell_length_b                   12.335(3)
_cell_length_c                   34.058(7)
_cell_measurement_reflns_used    17635
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4805
_cell_measurement_theta_min      1.6509
_cell_volume                     6952(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            24822
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.934
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.749
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0799
_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^)+(0.0001P)^2^+40.3269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                6875
_reflns_number_total             7920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00957_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        6952(2)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4088242