Reactions of [t-Bu2SnO]3 with [t-BuX2Si]2 (X = F, Cl). Syntheses and Structures of Novel Stannasiloxanes and of [(t-Bu2FSn)2O]2, the First Fluorine-Containing Tetraorganodistannoxane
Jens Beckmann; Monique Biesemans; Karl Hassler; Klaus Jurkschat; Jose C. Martins; Markus Schürmann; Rudolph Willem; Inorganic Chemistry 37 (1998) 4891–4897; doi:10.1021/ic971504+

data_4327682
_publ_section_title
;
 Reactions of [t-Bu2SnO]3 with [t-BuX2Si]2 (X = F, Cl). Syntheses and
 Structures of Novel Stannasiloxanes and of [(t-Bu2FSn)2O]2, the First
 Fluorine-Containing Tetraorganodistannoxane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4891
_journal_page_last               4897
_journal_paper_doi               10.1021/ic971504+
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C32 H72 F4 O4 Si4 Sn2'
_chemical_formula_sum            'C32 H72 F4 O4 Si4 Sn2'
_chemical_formula_weight         946.64
_chemical_melting_point          430
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                114.010(1)
_cell_angle_beta                 92.040(1)
_cell_angle_gamma                108.230(1)
_cell_formula_units_Z            1
_cell_length_a                   9.706(1)
_cell_length_b                   11.732(1)
_cell_length_c                   11.818(1)
_cell_measurement_reflns_used    13411
_cell_measurement_temperature    291(1)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      4.50
_cell_volume                     1146.82(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(1)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
; 
360 frames via \w-rotation (\D\w=1\%) and two times 10s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -110
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13411
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         4.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_meas      1.407(5)
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.949
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0774
_refine_ls_wR_factor_obs         0.0732
_reflns_number_observed          3033
_reflns_number_total             3998
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715042B_2.cif
_cod_data_source_block           (7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1146.8(2)
_cod_database_code               4327682