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_4107729
_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            'C29 H37 N5 O Sn3'
_chemical_formula_weight         827.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.630(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.331(3)
_cell_length_b                   17.970(4)
_cell_length_c                   15.809(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     3012.6(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34531
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  0.8853
_exptl_absorpt_correction_T_min  0.6760
_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 = 0.824829  

;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       'transparent needles'
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0362P)^2^+0.5751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                7010
_reflns_number_total             8804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801000b-file001.cif
_cod_data_source_block           sad
_cod_original_cell_volume        3012.5(11)
_cod_database_code               4107729