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_1545265
_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 Cl Pb Ru Si2'
_chemical_formula_sum            'C38 H55 Cl Pb Ru Si2'
_chemical_formula_weight         911.72
_chemical_name_systematic        ClOlumboleRuthenocene
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.419(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7280(12)
_cell_length_b                   18.602(2)
_cell_length_c                   21.538(3)
_cell_measurement_reflns_used    3877
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.22
_cell_volume                     3880.1(8)
_computing_cell_refinement       'Bruker SAINT (Bruker 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker 2008)'
_computing_data_reduction        'Bruker SAINT and XPREP (Bruker 2008)'
_computing_molecular_graphics    'XSHEL (Bruker, 2002)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19407
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP; Bruker AXS 2008'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.650
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                5281
_reflns_number_total             7476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc04843a2.cif
_cod_data_source_block           masa828
_cod_depositor_comments
'Adding full bibliography for 1545265--1545268.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1545265