Reactions of a Highly Crowded Cyclic Stannylene with Iodoalkanes, Enones, and Dienes. Inhibition of Nucleophilic Substitution at Tin(IV) Centers
Asadi, Ashrafolmolouk; Eaborn, Colin; Hill, Michael S.; Hitchcock, Peter B.; Meehan, Margaret M.; Smith, J. David; Organometallics 21 (2002) 2430–; doi:10.1021/om020106y

data_4089721
_publ_section_title
;
 Reactions of a Highly Crowded Cyclic Stannylene with Iodoalkanes, Enones,
 and Dienes. Inhibition of Nucleophilic Substitution at Tin(IV) Centers
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2430
_journal_paper_doi               10.1021/om020106y
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H57 F3 O2 Si6 Sn1'
_chemical_formula_structural     'C24 H57 F3 O2 Si6 Sn1'
_chemical_formula_sum            'C24 H57 F3 O2 Si6 Sn'
_chemical_formula_weight         721.93
_chemical_name_common
'[Sn(Et)(O2CCF3){C(SiMe3)2SiMe2CH2CH2SiMe2C(SiMe3)2}]'
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-09-13T11:05:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0509(9)
_cell_length_b                   9.31730(10)
_cell_length_c                   22.2269(6)
_cell_measurement_reflns_used    31301
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     7051.8(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29430
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.54
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.264(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11504
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+6.7172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                10065
_reflns_number_total             11504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020106y.cif
_cod_data_source_block           sep1400
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_original_formula_sum        'C24 H57 F3 O2 Si6 Sn1'
_cod_database_code               4089721