Coordination Chemistry of Cyclic Disilylated Stannylenes and Plumbylenes to Group 4 Metallocenes
Henning Arp; Judith Baumgartner; Christoph Marschner; Patrick Zark; Thomas Müller; Journal of the American Chemical Society 134 (2012) 10864–10875; doi:10.1021/ja301547x

data_4118164
_publ_section_title
;
 Coordination Chemistry of Cyclic Disilylated Stannylenes and Plumbylenes
 to Group 4 Metallocenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10864
_journal_page_last               10875
_journal_paper_doi               10.1021/ja301547x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C32 H73 P Pb Si8 Ti'
_chemical_formula_weight         968.68
_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                84.78(3)
_cell_angle_beta                 84.62(3)
_cell_angle_gamma                66.66(3)
_cell_formula_units_Z            2
_cell_length_a                   11.950(2)
_cell_length_b                   12.274(3)
_cell_length_c                   19.463(4)
_cell_measurement_reflns_used    12800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.522
_cell_measurement_theta_min      4.334
_cell_volume                     2605.0(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       '\w 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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20847
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    3.613
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needles
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.717
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+8.1051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                9714
_reflns_number_total             10470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301547x_si_002_4.cif
_cod_data_source_block           8_819j
_cod_original_cell_volume        2605.0(9)
_cod_database_code               4118164