{4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C6H2Sn}2: An Intramolecularly Coordinated Organotin(I) Compound with a Sn-Sn Single Bond, Its Disproportionation toward a Diorganostannylene and Elemental Tin, and Its Oxidation with PhI(OAc)2
Michael Wagner; Christina Dietz; Stefan Krabbe; Stephan G. Koller; Carsten Strohmann; Klaus Jurkschat; Inorganic Chemistry 51 (2012) 6851–6859; doi:10.1021/ic3005954

data_4329508
_publ_contact_author_address
;Lehrstuhl f\"ur Anorganische Chemie II
Technische Universit\"at Dortmund
44221 Dortmund
Germany
;
_publ_contact_author_email       klaus.jurkschat@tu-dortmund.de
_publ_contact_author_name        'Klaus Jurkschat'
_publ_section_title
;
 {4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C6H2Sn}2: An Intramolecularly Coordinated
 Organotin(I) Compound with a Sn-Sn Single Bond, Its Disproportionation
 toward a Diorganostannylene and Elemental Tin, and Its Oxidation with
 PhI(OAc)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6851
_journal_page_last               6859
_journal_paper_doi               10.1021/ic3005954
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H42 O8 P2 Sn'
_chemical_formula_sum            'C24 H42 O8 P2 Sn'
_chemical_formula_weight         639.21
_chemical_name_systematic
; 
[2,6-Bis(diisopropoxyphosphonyl)-4-tert-butyl]phenyltin acetate 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1722(9)
_cell_length_b                   16.9303(12)
_cell_length_c                   18.0365(13)
_cell_measurement_reflns_used    4748
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1350
_cell_measurement_theta_min      2.2992
_cell_volume                     3106.2(4)
_computing_cell_refinement
"'CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37'"
_computing_data_collection
"'CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37'"
_computing_data_reduction
"'CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37'"
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.1744
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18266
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.687
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5713
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.691
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0137P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3023
_reflns_number_total             5713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3005954_si_002_1.cif
_cod_data_source_block           compound4
_cod_database_code               4329508