Hydrolysis of (Me3SiCH2)PhSnCl2. Isomerisation of the dimeric tetraorganodistannoxane [(Me3SiCH2)Ph(Cl)SnOSn(Cl)Ph(CH2SiMe3)]2
Beckmann, Jens; Dakternieks, Dainis; Duthie, Andrew; Tiekink, Edward R. T.; Dalton Transactions  (2003) 755–; doi:10.1039/b211070a

data_7012462
_publ_section_title
;
 Hydrolysis of (Me3SiCH2)PhSnCl2. Isomerisation of the dimeric
 tetraorganodistannoxane [(Me3SiCH2)Ph(Cl)SnOSn(Cl)Ph(CH2SiMe3)]2
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              755
_journal_paper_doi               10.1039/b211070a
_journal_year                    2003
_chemical_formula_sum            'C40 H64 Cl4 O2 Si4 Sn4'
_chemical_formula_weight         1305.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                91.26(5)
_cell_angle_beta                 100.37(3)
_cell_angle_gamma                93.14(4)
_cell_formula_units_Z            3
_cell_length_a                   12.203(2)
_cell_length_b                   27.565(12)
_cell_length_c                   12.138(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173
_cell_measurement_theta_max      9.5
_cell_measurement_theta_min      7.2
_cell_volume                     4008(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03208
_diffrn_orient_matrix_UB_12      0.03274
_diffrn_orient_matrix_UB_13      0.03065
_diffrn_orient_matrix_UB_21      -0.00387
_diffrn_orient_matrix_UB_22      -0.01049
_diffrn_orient_matrix_UB_23      0.07762
_diffrn_orient_matrix_UB_31      0.07695
_diffrn_orient_matrix_UB_32      -0.01182
_diffrn_orient_matrix_UB_33      0.00762
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19237
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.23
_refine_diff_density_min         -2.46
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         18375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_gt           0.033
_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^)+(0.0273P)^2^+10.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.088
_reflns_number_gt                13001
_reflns_number_total             18375
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b211070a.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012462