Synthesis and reactivity of a ruthenocene-type complex bearing an aromatic π-ligand with the heaviest group 14 element
Nakada, Marisa; Kuwabara, Takuya; Furukawa, Shunsuke; Hada, Masahiko; Minoura, Mao; Saito, Masaichi; Chem. Sci. 8 (2017) 3092–; doi:10.1039/C6SC04843A

data_1545268
_publ_section_title
;
 Synthesis and reactivity of a ruthenocene-type complex bearing an
 aromatic \p-ligand with the heaviest group 14 element
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              3092
_journal_paper_doi               10.1039/C6SC04843A
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C38 H55 Pb Ru Si2, C16 H32 Li O4'
_chemical_formula_sum            'C54 H87 Li O4 Pb Ru Si2'
_chemical_formula_weight         1171.63
_chemical_name_systematic        'Anionic PlumboleRuthenocene'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                97.8360(10)
_cell_angle_beta                 96.9920(10)
_cell_angle_gamma                93.2610(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7785(7)
_cell_length_b                   14.3628(8)
_cell_length_c                   15.1226(9)
_cell_measurement_reflns_used    6636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.49
_cell_volume                     2721.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19140
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.452
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.949
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                10711
_reflns_number_total             12507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc04843a2.cif
_cod_data_source_block           masa784
_cod_depositor_comments
'Adding full bibliography for 1545265--1545268.cif.'
_cod_database_code               1545268