#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:06:16 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178934 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116358.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_4116358
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         'C5 H12 O4 Sn'
_chemical_formula_sum            'C5 H12 O4 Sn'
_chemical_formula_weight         254.84
_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'
_audit_creation_date             'wed Dec 23 17:30:18 1998'
_audit_creation_method           ' from TEXRAY.INF file '
_cell_angle_alpha                92.77(2)
_cell_angle_beta                 110.46(3)
_cell_angle_gamma                93.01(2)
_cell_formula_units_Z            2
_cell_length_a                   8.160(3)
_cell_length_b                   8.724(2)
_cell_length_c                   6.641(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.5
_cell_volume                     441.2(2)
_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
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      243.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.04135
_diffrn_orient_matrix_UB_12      -0.01388
_diffrn_orient_matrix_UB_13      -0.16079
_diffrn_orient_matrix_UB_21      0.00490
_diffrn_orient_matrix_UB_22      -0.11389
_diffrn_orient_matrix_UB_23      0.00848
_diffrn_orient_matrix_UB_31      -0.12437
_diffrn_orient_matrix_UB_32      -0.00887
_diffrn_orient_matrix_UB_33      -0.00618
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.010
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2170
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        -2.61
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, phillips & Mathews, 1968)'
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured '
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             248.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       0.113(8)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.655
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0380
_refine_ls_shift/su_mean         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = l/[σ²(Fo) + 0.00063|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                1978
_reflns_number_total             2027
_reflns_threshold_expression     '>2.0 sigma (I) '
_cod_data_source_file            ja9900499_2.cif
_cod_data_source_block           '[Me2Sn(OMe)(OCO2Me)]2'
_cod_database_code               4116358
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-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 0.29912(2) 0.46474(2) 0.03443(2) 0.03092(9) Uani 1.00 d
O(1) O 0.5427(3) 0.3773(2) 0.0921(4) 0.0341(5) Uani 1.00 d
O(2) O 0.2474(3) 0.2637(3) 0.1949(4) 0.0420(6) Uani 1.00 d
O(3) O -0.0199(4) 0.3439(3) 0.1157(5) 0.0499(7) Uani 1.00 d
O(4) O 0.0383(3) 0.1252(3) 0.2660(4) 0.0461(6) Uani 1.00 d
C(1) C 0.3353(4) 0.6199(4) 0.3026(5) 0.0393(8) Uani 1.00 d
C(2) C 0.1543(4) 0.3652(4) -0.2761(5) 0.0441(8) Uani 1.00 d
C(3) C 0.5767(6) 0.2210(4) 0.1212(8) 0.053(1) Uani 1.00 d
C(4) C 0.0874(5) 0.2515(4) 0.1851(5) 0.0387(8) Uani 1.00 d
C(5) C 0.1634(6) 0.0157(5) 0.3447(9) 0.064(1) Uani 1.00 d
H(1) H 0.4307 0.5909 0.4222 0.0472 Uiso 1.00 calc
H(2) H 0.3624 0.7207 0.2692 0.0472 Uiso 1.00 calc
H(3) H 0.2322 0.6173 0.3360 0.0472 Uiso 1.00 calc
H(4) H 0.0371 0.3421 -0.2874 0.0544 Uiso 1.00 calc
H(5) H 0.1592 0.4346 -0.3794 0.0544 Uiso 1.00 calc
H(6) H 0.2048 0.2727 -0.2994 0.0544 Uiso 1.00 calc
H(7) H 0.5486 0.1894 0.2418 0.0631 Uiso 1.00 calc
H(8) H 0.5043 0.1590 -0.0043 0.0631 Uiso 1.00 calc
H(9) H 0.6955 0.2078 0.1449 0.0631 Uiso 1.00 calc
H(10) H 0.1139 -0.0688 0.3956 0.0798 Uiso 1.00 calc
H(11) H 0.2016 -0.0227 0.2322 0.0798 Uiso 1.00 calc
H(12) H 0.2627 0.0621 0.4598 0.0798 Uiso 1.00 calc
O(1*) O 0.4573(3) 0.6227(2) -0.0921(4) 0.0341(5) Uani 1.00 d
Sn(1*) Sn 0.70088(2) 0.53526(2) -0.03443(2) 0.03092(9) Uani 1.00 d
C(3*) C 0.4233(6) 0.7790(4) -0.1212(8) 0.053(1) Uani 1.00 d
O(2*) O 0.7526(3) 0.7363(3) -0.1949(4) 0.0420(6) Uani 1.00 d
C(1*) C 0.6647(4) 0.3801(4) -0.3026(5) 0.0393(8) Uani 1.00 d
C(2*) C 0.8457(4) 0.6348(4) 0.2761(5) 0.0441(8) Uani 1.00 d
H(7*) H 0.4514 0.8106 -0.2418 0.0631 Uiso 1.00 calc
H(8*) H 0.4957 0.8410 0.0043 0.0631 Uiso 1.00 calc
H(9*) H 0.3045 0.7922 -0.1449 0.0631 Uiso 1.00 calc
C(4*) C 0.9126(5) 0.7485(4) -0.1851(5) 0.0387(8) Uani 1.00 d
H(1*) H 0.5693 0.4091 -0.4222 0.0472 Uiso 1.00 calc
H(2*) H 0.6376 0.2793 -0.2692 0.0472 Uiso 1.00 calc
H(3*) H 0.7678 0.3827 -0.3360 0.0472 Uiso 1.00 calc
H(4*) H 0.9629 0.6579 0.2874 0.0544 Uiso 1.00 calc
H(5*) H 0.8408 0.5654 0.3794 0.0544 Uiso 1.00 calc
H(6*) H 0.7952 0.7273 0.2994 0.0544 Uiso 1.00 calc
O(3*) O 1.0199(4) 0.6561(3) -0.1157(5) 0.0499(7) Uani 1.00 d
O(4*) O 0.9617(3) 0.8748(3) -0.2660(4) 0.0461(6) Uani 1.00 d
C(5*) C 0.8366(6) 0.9843(5) -0.3447(9) 0.064(1) Uani 1.00 d
H(10*) H 0.8861 1.0688 -0.3956 0.0798 Uiso 1.00 calc
H(11*) H 0.7984 1.0227 -0.2322 0.0798 Uiso 1.00 calc
H(12*) H 0.7373 0.9379 -0.4598 0.0798 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 0 -1
-1 1 -1
-1 2 -1
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) 71.70(9) 1_555 1_555 2_665 yes
O(1) Sn(1) O(2) 84.20(8) 1_555 1_555 1_555 yes
O(1) Sn(1) C(1) 104.9(1) 1_555 1_555 1_555 yes
O(1) Sn(1) C(2) 101.9(1) 1_555 1_555 1_555 yes
O(1) Sn(1) O(2) 155.89(9) 2_665 1_555 1_555 yes
O(1) Sn(1) C(1) 91.7(1) 2_665 1_555 1_555 yes
O(1) Sn(1) C(2) 92.0(1) 2_665 1_555 1_555 yes
O(2) Sn(1) C(1) 93.8(1) 1_555 1_555 1_555 yes
O(2) Sn(1) C(2) 93.7(1) 1_555 1_555 1_555 yes
C(1) Sn(1) C(2) 152.8(1) 1_555 1_555 1_555 yes
Sn(1) O(1) Sn(1) 108.30(9) 1_555 1_555 2_665 yes
Sn(1) O(1) C(3) 124.8(2) 1_555 1_555 1_555 yes
Sn(1) O(1) C(3) 122.4(2) 2_665 1_555 1_555 yes
Sn(1) O(2) C(4) 111.3(2) 1_555 1_555 1_555 yes
C(4) O(4) C(5) 117.9(3) 1_555 1_555 1_555 yes
Sn(1) C(1) H(1) 109.0(2) 1_555 1_555 1_555 no
Sn(1) C(1) H(2) 109.1(2) 1_555 1_555 1_555 no
Sn(1) C(1) H(3) 109.5(2) 1_555 1_555 1_555 no
H(1) C(1) H(2) 109.1(3) 1_555 1_555 1_555 no
H(1) C(1) H(3) 110.0(3) 1_555 1_555 1_555 no
H(2) C(1) H(3) 110.1(3) 1_555 1_555 1_555 no
Sn(1) C(2) H(4) 109.4(2) 1_555 1_555 1_555 no
Sn(1) C(2) H(5) 109.3(2) 1_555 1_555 1_555 no
Sn(1) C(2) H(6) 108.8(3) 1_555 1_555 1_555 no
H(4) C(2) H(5) 110.4(4) 1_555 1_555 1_555 no
H(4) C(2) H(6) 109.6(3) 1_555 1_555 1_555 no
H(5) C(2) H(6) 109.3(3) 1_555 1_555 1_555 no
O(1) C(3) H(7) 109.3(4) 1_555 1_555 1_555 no
O(1) C(3) H(8) 109.4(4) 1_555 1_555 1_555 no
O(1) C(3) H(9) 110.1(3) 1_555 1_555 1_555 no
H(7) C(3) H(8) 108.5(4) 1_555 1_555 1_555 no
H(7) C(3) H(9) 109.8(4) 1_555 1_555 1_555 no
H(8) C(3) H(9) 109.7(4) 1_555 1_555 1_555 no
O(2) C(4) O(3) 125.9(3) 1_555 1_555 1_555 yes
O(2) C(4) O(4) 116.1(3) 1_555 1_555 1_555 yes
O(3) C(4) O(4) 117.9(3) 1_555 1_555 1_555 yes
O(4) C(5) H(10) 110.6(4) 1_555 1_555 1_555 no
O(4) C(5) H(11) 110.1(4) 1_555 1_555 1_555 no
O(4) C(5) H(12) 110.1(4) 1_555 1_555 1_555 no
H(10) C(5) H(11) 108.5(4) 1_555 1_555 1_555 no
H(10) C(5) H(12) 108.9(5) 1_555 1_555 1_555 no
H(11) C(5) H(12) 108.6(4) 1_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) 2.082(2) 1_555 1_555 yes
Sn(1) O(1) 2.226(2) 1_555 2_665 yes
Sn(1) O(2) 2.192(2) 1_555 1_555 yes
Sn(1) C(1) 2.109(3) 1_555 1_555 yes
Sn(1) C(2) 2.102(3) 1_555 1_555 yes
O(1) C(3) 1.415(4) 1_555 1_555 yes
O(2) C(4) 1.283(4) 1_555 1_555 yes
O(3) C(4) 1.207(4) 1_555 1_555 yes
O(4) C(4) 1.352(4) 1_555 1_555 yes
O(4) C(5) 1.416(5) 1_555 1_555 yes
C(1) H(1) 0.953 1_555 1_555 no
C(1) H(2) 0.951 1_555 1_555 no
C(1) H(3) 0.941 1_555 1_555 no
C(2) H(4) 0.943 1_555 1_555 no
C(2) H(5) 0.946 1_555 1_555 no
C(2) H(6) 0.955 1_555 1_555 no
C(3) H(7) 0.955 1_555 1_555 no
C(3) H(8) 0.956 1_555 1_555 no
C(3) H(9) 0.941 1_555 1_555 no
C(5) H(10) 0.954 1_555 1_555 no
C(5) H(11) 0.958 1_555 1_555 no
C(5) H(12) 0.953 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
Sn(1) O(3) 2.818(3) 1_555 2_565
O(1) O(3) 3.545(4) 1_555 1_655
O(3) C(1) 3.100(4) 1_555 2_565
O(3) C(2) 3.102(5) 1_555 2_565
O(3) O(3) 3.247(6) 1_555 2_565
O(3) C(3) 3.421(4) 1_555 1_455
O(4) C(2) 3.419(4) 1_555 1_556
C(2) C(4) 3.510(4) 1_555 1_554
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 2_665 2_665 yes
Sn(1) O(1) Sn(1) O(2) -1.7(3) 1_555 1_555 2_665 2_665 yes
Sn(1) O(1) Sn(1) C(1) -l05.1(1) 1_555 1_555 2_665 2_665 yes
Sn(1) O(1) Sn(1) C(2) 101.9(1) 1_555 1_555 2_665 2_665 yes
Sn(1) O(1) Sn(1) O(1) 0.0 1_555 2_665 2_665 1_555 yes
Sn(1) O(1) Sn(1) O(2) 179.3(1) 1_555 2_665 2_665 2_665 yes
Sn(1) O(1) Sn(1) C(1) 86.9(1) 1_555 2_665 2_665 2_665 yes
Sn(1) O(1) Sn(1) C(2) -88.1(1) 1_555 2_665 2_665 2_665 yes
Sn(1) O(2) C(4) O(3) -6.5(4) 1_555 1_555 1_555 1_555 yes
Sn(1) O(2) C(4) O(4) 175.5(2) 1_555 1_555 1_555 1_555 yes
O(1) Sn(1) O(1) Sn(1) 0.0 1_555 1_555 2_665 2_665 yes
O(1) Sn(1) O(1) C(3) -157.0(3) 1_555 1_555 2_665 2_665 yes
O(1) Sn(1) O(2) C(4) -173.3(2) 1_555 1_555 1_555 1_555 yes
O(1) Sn(1) O(1) Sn(1) 0.0 1_555 2_665 2_665 1_555 yes
O(1) Sn(1) O(1) C(3) 156.3(3) 1_555 2_665 2_665 2_665 yes
O(1) Sn(1) O(2) C(4) 175.0(2) 1_555 2_665 2_665 2_665 yes
O(2) Sn(1) O(1) C(3) 24.4(3) 1_555 1_555 1_555 1_555 yes
O(2) Sn(1) O(1) C(3) -155.3(3) 1_555 1_555 2_665 2_665 yes
O(2) C(4) O(4) C(5) -2.7(5) 1_555 1_555 1_555 1_555 yes
O(3) C(4) O(4) C(5) 179.1(4) 1_555 1_555 1_555 l_555 yes
C(1) Sn(1) O(1) C(3) 116.8(3) 1_555 1_555 1_555 1_555 yes
C(1) Sn(1) O(1) C(3) -51.9(3) 1_555 1_555 2_665 2_665 yes
C(1) Sn(1) O(2) C(4) 82.0(2) 1_555 1_555 1_555 1_555 yes
C(2) Sn(1) O(1) C(3) -68.2(3) 1_555 1_555 1_555 1_555 yes
C(2) Sn(1) O(1) C(3) 101.1(3) 1_555 1_555 2_665 2_665 yes
C(2) Sn(1) O(2) C(4) -71.8(2) 1_555 1_555 1_55S 1_555 yes
