Dispersion Energy Enforced Dimerization of a Cyclic Disilylated Plumbylene
Henning Arp; Judith Baumgartner; Christoph Marschner; Patrick Zark; Thomas Müller; Journal of the American Chemical Society 134 (2012) 6409–6415; doi:10.1021/ja300654t

data_4117785
_publ_section_title
;
 Dispersion Energy Enforced Dimerization of a Cyclic Disilylated
 Plumbylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6409
_journal_page_last               6415
_journal_paper_doi               10.1021/ja300654t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C34 H48 B F15 Pb Si8'
_chemical_formula_weight         1184.44
_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                81.96(3)
_cell_angle_beta                 74.89(3)
_cell_angle_gamma                61.25(3)
_cell_formula_units_Z            2
_cell_length_a                   11.896(2)
_cell_length_b                   12.182(2)
_cell_length_c                   20.051(4)
_cell_measurement_reflns_used    9358
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.523
_cell_measurement_theta_min      4.954
_cell_volume                     2459.1(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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0663
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19515
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    3.707
_exptl_absorpt_correction_T_max  0.6646
_exptl_absorpt_correction_T_min  0.3488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       plates
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.361
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0688P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                8754
_reflns_number_total             9890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300654t_si_002_2.cif
_cod_data_source_block           3_812j
_cod_original_cell_volume        2459.1(8)
_cod_database_code               4117785