#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/77/2237748.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2237748
loop_
_publ_author_name
'Reichelt, Martin'
'Reuter, Hans'
_publ_section_title
;
 Diacetatodi-tert-butyltin(IV)
;
_journal_coeditor_code           AA2086
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m254
_journal_paper_doi               10.1107/S1600536813009185
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Sn (C4 H9)2 (C2 H3 O2)2]'
_chemical_formula_moiety         'C12 H24 O4 Sn'
_chemical_formula_sum            'C12 H24 O4 Sn'
_chemical_formula_weight         351.00
_chemical_name_systematic
;
Diacetatodi-tert-butyltin(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.462(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1039(3)
_cell_length_b                   15.3928(7)
_cell_length_c                   15.9601(8)
_cell_measurement_reflns_used    6480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.56
_cell_volume                     1492.74(12)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and Mercury
(Macrae et al., 2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76636
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.9393
_exptl_absorpt_correction_T_min  0.7905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.507
_refine_ls_extinction_coef       0.00201(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0133P)²+1.0511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                2980
_reflns_number_total             3590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            aa2086.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2237748
_cod_database_fobs_code          2237748
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Sn Sn1 0.19140(2) 0.295768(9) 0.285075(8) 0.01333(6) Uani d . 1 1
C C11 0.0432(3) 0.20445(14) 0.19231(13) 0.0162(4) Uani d . 1 1
C C12 -0.1709(3) 0.24192(16) 0.14968(14) 0.0257(5) Uani d . 1 1
H H12A -0.2374 0.2001 0.1085 0.031(2) Uiso calc R 1 1
H H12B -0.1396 0.2962 0.1211 0.031(2) Uiso calc R 1 1
H H12C -0.2730 0.2534 0.1922 0.031(2) Uiso calc R 1 1
C C13 0.2095(4) 0.18975(15) 0.12781(13) 0.0216(5) Uani d . 1 1
H H13A 0.3485 0.1689 0.1566 0.031(2) Uiso calc R 1 1
H H13B 0.2350 0.2445 0.0990 0.031(2) Uiso calc R 1 1
H H13C 0.1515 0.1464 0.0865 0.031(2) Uiso calc R 1 1
C C14 -0.0036(4) 0.11881(15) 0.23553(14) 0.0259(5) Uani d . 1 1
H H14A -0.1128 0.1285 0.2758 0.031(2) Uiso calc R 1 1
H H14B 0.1327 0.0966 0.2654 0.031(2) Uiso calc R 1 1
H H14C -0.0609 0.0764 0.1932 0.031(2) Uiso calc R 1 1
C C21 0.0894(3) 0.38924(14) 0.37595(12) 0.0161(4) Uani d . 1 1
C C22 -0.0723(4) 0.34722(15) 0.43092(14) 0.0245(5) Uani d . 1 1
H H22A -0.1180 0.3900 0.4713 0.030(2) Uiso calc R 1 1
H H22B -0.0011 0.2980 0.4614 0.030(2) Uiso calc R 1 1
H H22C -0.2016 0.3267 0.3953 0.030(2) Uiso calc R 1 1
C C23 0.2995(4) 0.41692(15) 0.42919(14) 0.0243(5) Uani d . 1 1
H H23A 0.2626 0.4591 0.4717 0.030(2) Uiso calc R 1 1
H H23B 0.4014 0.4435 0.3928 0.030(2) Uiso calc R 1 1
H H23C 0.3689 0.3659 0.4572 0.030(2) Uiso calc R 1 1
C C24 -0.0185(4) 0.46712(15) 0.33009(14) 0.0249(5) Uani d . 1 1
H H24A -0.1502 0.4481 0.2950 0.030(2) Uiso calc R 1 1
H H24B 0.0852 0.4936 0.2944 0.030(2) Uiso calc R 1 1
H H24C -0.0601 0.5098 0.3713 0.030(2) Uiso calc R 1 1
O O11 0.4677(2) 0.22581(9) 0.33641(9) 0.0198(3) Uani d . 1 1
O O12 0.1995(3) 0.18113(10) 0.40892(10) 0.0251(4) Uani d . 1 1
C C15 0.3940(4) 0.17649(14) 0.39399(13) 0.0203(5) Uani d . 1 1
C C16 0.5546(4) 0.11407(16) 0.43777(14) 0.0265(5) Uani d . 1 1
H H16A 0.5282 0.1099 0.4973 0.037(4) Uiso calc R 1 1
H H16B 0.7049 0.1347 0.4333 0.037(4) Uiso calc R 1 1
H H16C 0.5357 0.0567 0.4114 0.037(4) Uiso calc R 1 1
O O21 0.4416(2) 0.36282(9) 0.23048(9) 0.0178(3) Uani d . 1 1
O O22 0.1404(2) 0.41038(10) 0.15759(9) 0.0231(3) Uani d . 1 1
C C25 0.3440(4) 0.40733(13) 0.16819(13) 0.0185(5) Uani d . 1 1
C C26 0.4899(4) 0.45081(15) 0.11080(14) 0.0240(5) Uani d . 1 1
H H26A 0.5160 0.4114 0.0646 0.038(4) Uiso calc R 1 1
H H26B 0.6306 0.4656 0.1423 0.038(4) Uiso calc R 1 1
H H26C 0.4188 0.5039 0.0879 0.038(4) Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O21 Sn1 O11 79.93(6)
O21 Sn1 C11 107.88(7)
O11 Sn1 C11 101.58(7)
O21 Sn1 C21 102.54(7)
O11 Sn1 C21 110.43(7)
C11 Sn1 C21 138.97(7)
C14 C11 C12 109.77(18)
C14 C11 C13 109.93(18)
C12 C11 C13 110.51(17)
C14 C11 Sn1 109.51(14)
C12 C11 Sn1 109.99(14)
C13 C11 Sn1 107.09(13)
C11 C12 H12A 109.5
C11 C12 H12B 109.5
H12A C12 H12B 109.5
C11 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C11 C13 H13A 109.5
C11 C13 H13B 109.5
H13A C13 H13B 109.5
C11 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C11 C14 H14A 109.5
C11 C14 H14B 109.5
H14A C14 H14B 109.5
C11 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
C24 C21 C22 109.65(17)
C24 C21 C23 110.46(18)
C22 C21 C23 110.65(17)
C24 C21 Sn1 109.79(13)
C22 C21 Sn1 110.17(14)
C23 C21 Sn1 106.07(13)
C21 C22 H22A 109.5
C21 C22 H22B 109.5
H22A C22 H22B 109.5
C21 C22 H22C 109.5
H22A C22 H22C 109.5
H22B C22 H22C 109.5
C21 C23 H23A 109.5
C21 C23 H23B 109.5
H23A C23 H23B 109.5
C21 C23 H23C 109.5
H23A C23 H23C 109.5
H23B C23 H23C 109.5
C21 C24 H24A 109.5
C21 C24 H24B 109.5
H24A C24 H24B 109.5
C21 C24 H24C 109.5
H24A C24 H24C 109.5
H24B C24 H24C 109.5
C15 O11 Sn1 104.81(13)
O12 C15 O11 120.3(2)
O12 C15 C16 123.1(2)
O11 C15 C16 116.6(2)
C15 C16 H16A 109.5
C15 C16 H16B 109.5
H16A C16 H16B 109.5
C15 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
C25 O21 Sn1 106.07(13)
O22 C25 O21 120.25(19)
O22 C25 C26 123.21(19)
O21 C25 C26 116.51(19)
C25 C26 H26A 109.5
C25 C26 H26B 109.5
H26A C26 H26B 109.5
C25 C26 H26C 109.5
H26A C26 H26C 109.5
H26B C26 H26C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 O21 2.1001(14) yes
Sn1 O11 2.1002(14) yes
Sn1 C11 2.175(2) yes
Sn1 C21 2.176(2) yes
C11 C14 1.527(3) ?
C11 C12 1.528(3) ?
C11 C13 1.530(3) ?
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
C13 H13A 0.9800 ?
C13 H13B 0.9800 ?
C13 H13C 0.9800 ?
C14 H14A 0.9800 ?
C14 H14B 0.9800 ?
C14 H14C 0.9800 ?
C21 C24 1.522(3) ?
C21 C22 1.525(3) ?
C21 C23 1.530(3) ?
C22 H22A 0.9800 ?
C22 H22B 0.9800 ?
C22 H22C 0.9800 ?
C23 H23A 0.9800 ?
C23 H23B 0.9800 ?
C23 H23C 0.9800 ?
C24 H24A 0.9800 ?
C24 H24B 0.9800 ?
C24 H24C 0.9800 ?
O11 C15 1.304(3) yes
O12 C15 1.235(3) yes
C15 C16 1.497(3) ?
C16 H16A 0.9800 ?
C16 H16B 0.9800 ?
C16 H16C 0.9800 ?
O21 C25 1.304(3) yes
O22 C25 1.239(3) yes
C25 C26 1.495(3) ?
C26 H26A 0.9800 ?
C26 H26B 0.9800 ?
C26 H26C 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C12 H12C O21 1_455 0.98 2.54 3.362(3) 141.5
C22 H22C O11 1_455 0.98 2.65 3.584(3) 160.0
C16 H16C O22 2_545 0.98 2.69 3.636(3) 163.2
C16 H16A O22 4_666 0.98 2.60 3.518(3) 155.2
