A Reversible Valence Equilibrium in a Heavier Main Group Compound
Andrew D. Phillips; Shirley Hino; Philip P. Power; Journal of the American Chemical Society 125 (2003) 7520–7521; doi:10.1021/ja0347843

data_4113833
_publ_section_title
;
 A Reversible Valence Equilibrium in a Heavier Main Group Compound
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7520
_journal_page_last               7521
_journal_paper_doi               10.1021/ja0347843
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C96 H136 Sn2'
_chemical_formula_weight         1527.43
_chemical_name_common            Bert*SnSnPh2Bert*.2C6H14
_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                109.107(6)
_cell_angle_beta                 90.280(6)
_cell_angle_gamma                110.262(5)
_cell_formula_units_Z            2
_cell_length_a                   12.5615(15)
_cell_length_b                   17.893(3)
_cell_length_c                   21.802(3)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.197
_cell_measurement_theta_min      2.429
_cell_volume                     4305.0(11)
_computing_cell_refinement       'Bruker SAINT 6.33B (Bruker 2002)'
_computing_data_collection       'Bruker SMART 5.054 (Bruker 2002)'
_computing_data_reduction        'Bruker SAINT 6.33B (Bruker 2002)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39027
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time
;
frames measured at beginning and end of data collection
;
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.04 (Bruker 2002)'
_exptl_crystal_colour            teal
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0318P)^2^+4.0136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                12505
_reflns_number_total             15477
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ja0347843si20030220_031551.cif
_cod_data_source_block           adp75
_cod_original_cell_volume        4304.9(10)
_cod_database_code               4113833