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#$Date: 2016-03-22 12:06:16 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178934 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116357.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116357
loop_
_publ_author_name
'Jun-Chul Choi'
'Toshiyasu Sakakura'
'Takeshi Sako'
_publ_contact_author_address
;
National Institute of Materials and Chemical Research, 1-1 Higashi,
Tsukuba, Ibaraki 305-8565, Japan
;
_publ_contact_author_email       sakakura@home.nimc.go.jp
_publ_contact_author_fax         81-298-54-4687
_publ_contact_author_name        'Dr. Toshiyasu Sakakura'
_publ_contact_author_phone       81-298-54-4688
_publ_section_title
;
 Reaction of Dialkyltin Methoxide with Carbon Dioxide Relevant to the
 Mechanism of Catalytic Carbonate Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3793
_journal_page_last               3794
_journal_paper_doi               10.1021/ja9900499
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C4 H12 O2 Sn'
_chemical_formula_sum            'C4 H12 O2 Sn'
_chemical_formula_weight         210.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Dec 18 17:Ol:17 1998'
_audit_creation_method           ' from TEXRAY.INF file '
_cell_angle_alpha                90.02(7)
_cell_angle_beta                 91.78(8)
_cell_angle_gamma                89.98(10)
_cell_formula_units_Z            4
_cell_length_a                   8.03(1)
_cell_length_b                   8.162(6)
_cell_length_c                   11.375(8)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    243.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     745.2(12)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      243.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.02914
_diffrn_orient_matrix_UB_12      -0.11911
_diffrn_orient_matrix_UB_13      0.00184
_diffrn_orient_matrix_UB_21      -0.03197
_diffrn_orient_matrix_UB_22      -0.00586
_diffrn_orient_matrix_UB_23      0.08416
_diffrn_orient_matrix_UB_31      -0.11677
_diffrn_orient_matrix_UB_32      -0.02809
_diffrn_orient_matrix_UB_33      -0.02549
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1825
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        -5.13
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.341
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, phillips & Mathews, 1968)'
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured '
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             408.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.64
_refine_diff_density_min         -1.46
_refine_ls_extinction_coef       0.010(4)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.860
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0790
_refine_ls_shift/su_mean         0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00123|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                1332
_reflns_number_total             1722
_reflns_threshold_expression     '>2.0 sigma (I) '
_cod_data_source_file            ja9900499_1.cif
_cod_data_source_block           '[Me2Sn(OMe)2]2'
_cod_original_cell_volume        745(1)
_cod_database_code               4116357
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
Sn(1) Sn 0.37349(7) 0.07898(6) 0.87953(4) 0.0502(2) Uani 1.00 d
O(1) O 0.3976(8) -0.1133(6) 0.9930(5) 0.058(2) Uani 1.00 d
O(2) O 0.1771(9) -0.0244(10) 0.7893(6) 0.075(2) Uani 1.00 d
C(1) C 0.547(1) 0.056(1) 0.7435(8) 0.062(2) Uani 1.00 d
C(2) C 0.257(1) 0.279(1) 0.9656(7) 0.061(2) Uani 1.00 d
C(3) C 0.293(1) -0.257(1) 0.9846(8) 0.079(3) Uani 1.00 d
C(4) C 0.023(2) 0.019(1) 0.7994(10) 0.083(3) Uani 1.00 d
H(1) H 0.5581 -0.0568 0.7231 0.0746 Uiso 1.00 calc
H(2) H 0.5065 0.1146 0.6757 0.0746 Uiso 1.00 calc
H(3) H 0.6509 0.0984 0.7687 0.0746 Uiso 1.00 calc
H(4) H 0.3366 0.3399 1.0116 0.0761 Uiso 1.00 calc
H(5) H 0.2054 0.3513 0.9090 0.0761 Uiso 1.00 calc
H(6) H 0.1727 0.2400 1.0163 0.0761 Uiso 1.00 calc
H(7) H 0.1792 -0.2315 0.9917 0.1000 Uiso 1.00 calc
H(8) H 0.3077 -0.3121 0.9106 0.1000 Uiso 1.00 calc
H(9) H 0.3248 -0.3342 1.0459 0.1000 Uiso 1.00 calc
H(10) H 0.0073 0.1319 0.7802 0.1027 Uiso 1.00 calc
H(11) H -0.0497 -0.0454 0.7508 0.1027 Uiso 1.00 calc
H(12) H -0.0109 0.0048 0.8804 0.1027 Uiso 1.00 calc
O(1*) O 0.6024(8) 0.1133(6) 1.0070(5) 0.058(2) Uani 1.00 d
Sn(1*) Sn 0.62651(7) -0.07898(6) 1.12047(4) 0.0502(2) Uani 1.00 d
C(3*) C 0.707(1) 0.257(1) 1.0154(8) 0.079(3) Uani 1.00 d
O(2*) O 0.8229(9) 0.0244(10) 1.2107(6) 0.075(2) Uani 1.00 d
C(1*) C 0.453(1) -0.056(1) 1.2565(8) 0.062(2) Uani 1.00 d
C(2*) C 0.743(1) -0.279(1) 1.0344(7) 0.061(2) Uani 1.00 d
H(7*) H 0.8208 0.2315 1.0083 0.1000 Uiso 1.00 calc
H(8*) H 0.6923 0.3121 1.0894 0.1000 Uiso 1.00 calc
H(9*) H 0.6752 0.3342 0.9541 0.1000 Uiso 1.00 calc
C(4*) C 0.977(2) -0.019(1) 1.2006(10) 0.083(3) Uani 1.00 d
H(1*) H 0.4419 0.0568 1.2769 0.0746 Uiso 1.00 calc
H(2*) H 0.4935 -0.1146 1.3243 0.0746 Uiso 1.00 calc
H(3*) H 0.3491 -0.0984 1.2313 0.0746 Uiso 1.00 calc
H(4*) H 0.6634 -0.3399 0.9884 0.0761 Uiso 1.00 calc
H(5*) H 0.7946 -0.3513 1.0910 0.0761 Uiso 1.00 calc
H(6*) H 0.8273 -0.2400 0.9837 0.0761 Uiso 1.00 calc
H(10*) H 0.9927 -0.1319 1.2198 0.1027 Uiso 1.00 calc
H(11*) H 1.0497 0.0454 1.2492 0.1027 Uiso 1.00 calc
H(12*) H 1.0109 -0.0048 1.1196 0.1027 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography 
 (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
H H 0.000 0.000
;International Tables for Crystallography 
(1992, Vol. C, Table 6.1.1.2) 
;
O O 0.011 0.006
;International Tables for Crystallography 
 (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
;
Sn Sn -0.654 1.425
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2,6.8 and 6,1,1,1) 
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 -1 0
0 -1 -2
0 -1 2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Sn(1) O(1) 68.9(2) 1_555 1_555 3_657 yes
O(1) Sn(1) O(2) 93.2(3) 1_555 1_555 1_555 yes
O(1) Sn(1) C(1) 110.0(3) 1_555 1_555 1_555 yes
O(1) Sn(1) C(2) 109.4(3) 1_555 1_555 1_555 yes
O(1) Sn(1) O(2) 161.7(3) 3_657 1_555 1_555 yes
O(1) Sn(1) C(1) 86.6(3) 3_657 1_555 1_555 yes
O(1) Sn(1) C(2) 88.3(3) 3_657 1_555 1_555 yes
O(2) Sn(1) C(1) 96.4(3) 1_555 1_555 1_555 yes
O(2) Sn(1) C(2) 101.8(3) 1_555 1_555 1_555 yes
C(1) Sn(1) C(2) 135.1(3) 1_555 1_555 1_555 yes
Sn(1) O(1) Sn(1) 111.1(2) 1_555 1_555 3_657 yes
Sn(1) O(1) C(3) 122.8(5) 1_555 1_555 1_555 yes
Sn(1) O(1) C(3) 125.8(5) 3_657 1_555 1_555 yes
Sn(1) O(2) C(4) 124.6(7) 1_555 1_555 1_555 yes
Sn(1) C(1) H(1) 109.4(7) 1_555 1_555 1_555 no
Sn(1) C(1) H(2) 109.4(7) 1_555 1_555 1_555 no
Sn(1) C(1) H(3) 110.1(6) 1_555 1_555 1_555 no
H(1) C(1) H(2) 108.5(8) 1_555 1_555 1_555 no
H(1) C(1) H(3) 109.7(9) 1_555 1_555 1_555 no
H(2) C(1) H(3) 109.7(9) 1_555 1_555 1_555 no
Sn(1) C(2) H(4) 111.1(7) 1_555 1_555 1_555 no
Sn(1) C(2) H(5) 110.6(6) 1_555 1_555 1_555 no
Sn(1) C(2) H(6) 110.7(6) 1_555 1_555 1_555 no
H(4) C(2) H(5) 108.3(8) 1_555 1_555 1_555 no
H(4) C(2) H(6) 108.4(8) 1_555 1_555 1_555 no
H(5) C(2) H(6) 107.7(9) 1_555 1_555 1_555 no
O(1) C(3) H(7) 112.0(8) 1_555 1_555 1_555 no
O(1) C(3) H(8) 110.5(9) 1_555 1_555 1_555 no
O(1) C(3) H(9) 110.0(7) 1_555 1_555 1_555 no
H(7) C(3) H(8) 108.7(8) 1_555 1_555 1_555 no
H(7) C(3) H(9) 108(1) 1_555 1_555 1_555 no
H(8) C(3) H(9) 107.0(9) 1_555 1_555 1_555 no
O(2) C(4) H(10) 111(1) 1_555 1_555 1_555 no
O(2) C(4) H(11) 111(1) 1_555 1_555 1_555 no
O(2) C(4) H(12) 110.2(10) 1_555 1_555 1_555 no
H(10) C(4) H(11) 109(1) 1_555 1_555 1_555 no
H(10) C(4) H(12) 107(1) 1_555 1_555 1_555 no
H(11) C(4) H(12) 107(1) l_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn(1) O(1) 2.038(5) 1_555 1_555 yes
Sn(1) O(1) 2.324(6) 1_555 3_657 yes
Sn(1) O(2) 2.038(7) 1_555 1_555 yes
Sn(1) C(1) 2.121(9) 1_555 1_555 yes
Sn(1) C(2) 2.130(8) 1_555 1_555 yes
O(1) C(3) 1.445(10) 1_555 1_555 yes
O(2) C(4) 1.30(1) 1_555 1_555 yes
C(1) H(1) 0.956 1_555 1_555 no
C(1) H(2) 0.956 1_555 1_555 no
C(1) H(3) 0.941 1_555 1_555 no
C(2) H(4) 0.953 1_555 1_555 no
C(2) H(5) 0.962 1_555 1_555 no
C(2) H(6) 0.960 1_555 1_555 no
C(3) H(7) 0.946 1_555 1_555 no
C(3) H(8) 0.963 1_555 1_555 no
C(3) H(9) 0.966 1_555 1_555 no
C(4) H(10) 0.951 1_555 1_555 no
C(4) H(11) 0.952 1_555 1_555 no
C(4) H(12) 0.977 1_555 1_555 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
O(2) C(2) 3.370(10) 1_555 2_546
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sn(1) O(1) Sn(1) O(1) 0.0 1_555 1_555 3_657 3_657 yes
Sn(1) O(1) Sn(1) O(2) 12.7(10) 1_555 1_555 3_657 3_657 yes
Sn(1) O(1) Sn(1) C(1) 113.0(4) 1_555 1_555 3_657 3_657 yes
Sn(1) O(1) Sn(1) C(2) -111.6(3) 1_555 1_555 3_657 3_657 yes
Sn(1) O(1) Sn(1) O(1) 0.0 1_555 3_657 3_657 1_555 yes
Sn(1) O(1) Sn(1) O(2) -176.0(3) 1_555 3_657 3_657 3_657 yes
Sn(1) O(1) Sn(1) C(1) -78.0(4) 1_555 3_657 3_657 3_657 yes
Sn(1) O(1) Sn(1) C(2) 80.2(4) 1_555 3_657 3_657 3_657 yes
O(1) Sn(1) O(1) Sn(1) 0.0 1_555 1_555 3_657 3_657 yes
O(1) Sn(1) O(1) C(3) -174.2(9) 1_555 1_555 3_657 3_657 yes
O(1) Sn(1) O(2) C(4) 103.8(9) 1_555 1_555 1_555 1_555 yes
O(1) Sn(1) O(1) Sn(1) 0.0 1_555 3_657 3_657 1_555 yes
O(1) Sn(1) O(1) C(3) 174.4(9) 1_555 3_657 3_657 3_657 yes
O(1) Sn(1) O(2) C(4) -115(1) 1_555 3_657 3_657 3_657 yes
O(2) Sn(1) O(1) C(3) 1.7(8) 1_555 1_555 1_555 1_555 yes
O(2) Sn(1) O(1) C(3) 173.1(9) 1_555 1_555 3_657 3_657 yes
C(1) Sn(1) O(1) C(3) -96.4(8) 1_555 1_555 1_555 1_555 yes
C(1) Sn(1) O(1) C(3) 72.8(8) 1_555 1_555 3_657 3_657 yes
C(1) Sn(1) O(2) C(4) -145.6(9) 1_555 1_555 1_555 1_555 yes
C(2) Sn(1) O(1) C(3) 105.4(8) 1_555 1_555 1_555 1_555 yes
C(2) Sn(1) O(1) C(3) -62.6(8) 1_555 1_555 3_657 3_657 yes
C(2) Sn(1) O(2) C(4) -6.8(9) 1_555 1_555 1_555 1_555 yes
