Trapping of Tin(II) and Lead(II) Homologues of Carbon Monoxide by a Benzannulated Lutidine-Bridged Bisstannylene
Alexander V. Zabula; Tania Pape; Alexander Hepp; Falko M. Schappacher; Ute Ch. Rodewald; Rainer Pöttgen; F. Ekkehardt Hahn; Journal of the American Chemical Society 130 (2008) 5648–5649; doi:10.1021/ja801000b

data_4107730
_publ_section_title
;
 Trapping of Tin(II) and Lead(II) Homologues of Carbon Monoxide by a
 Benzannulated Lutidine-Bridged Bisstannylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5648
_journal_page_last               5649
_journal_paper_doi               10.1021/ja801000b
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C32.5 H44.5 N5 O1.5 Pb Sn2'
_chemical_formula_weight         973.80
_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                114.633(2)
_cell_angle_beta                 112.534(2)
_cell_angle_gamma                91.377(2)
_cell_formula_units_Z            4
_cell_length_a                   13.9440(16)
_cell_length_b                   17.450(2)
_cell_length_c                   18.007(2)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     3589.5(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35386
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    6.092
_exptl_absorpt_correction_T_max  0.7927
_exptl_absorpt_correction_T_min  0.5285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =  0.704388 

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             1874
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.851
_refine_diff_density_min         -2.443
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         16473
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0625P)^2^+5.0221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                12386
_reflns_number_total             16473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801000b-file002.cif
_cod_data_source_block           sad
_cod_original_formula_sum        'C32.50 H44.50 N5 O1.50 Pb Sn2'
_cod_database_code               4107730