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_1545266
_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 I Pb Ru Si2, C6 H14'
_chemical_formula_sum            'C44 H69 I Pb Ru Si2'
_chemical_formula_weight         1089.33
_chemical_name_systematic        IodoPlumboleRuthenocene
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_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
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.3930(5)
_cell_length_b                   22.3163(10)
_cell_length_c                   39.5129(17)
_cell_measurement_reflns_used    6602
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.22
_cell_volume                     9164.4(7)
_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 0.998
_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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            61813
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.752
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10525
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+24.9284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                8138
_reflns_number_total             10525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc04843a2.cif
_cod_data_source_block           masa796i
_cod_depositor_comments
'Adding full bibliography for 1545265--1545268.cif.'
_cod_database_code               1545266