#------------------------------------------------------------------------------
#$Date: 2016-03-21 15:03:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178735 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/46/4084638.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_4084638
loop_
_publ_author_name
'Wang, Lingfang'
'Kefalidis, Christos E.'
'Roisnel, Thierry'
'Sinbandhit, Sourisak'
'Maron, Laurent'
'Carpentier, Jean-François'
'Sarazin, Yann'
_publ_section_title
;
 Structure vs119Sn NMR Chemical Shift in Three-Coordinated Tin(II)
 Complexes: Experimental Data and Predictive DFT Computations
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2139
_journal_paper_doi               10.1021/om5007566
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 H14 Cl2 O2 Sn2'
_chemical_formula_sum            'C6 H14 Cl2 O2 Sn2'
_chemical_formula_weight         426.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2013-04-23T16:00:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.8330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6503(3)
_cell_length_b                   10.2650(4)
_cell_length_c                   9.0775(3)
_cell_measurement_reflns_used    3277
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.05
_cell_measurement_wavelength     0.71073
_cell_volume                     599.03(4)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5006
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    4.580
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0410P)²+0.5435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                1310
_reflns_number_total             1368
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details
;
 .res file for SHELXL : job.res
.................................................................
TITL import in P 21/a
CELL  0.71073   6.6503  10.2650   9.0775   90.000  104.833   90.000
ZERR     2.00   0.0003   0.0004   0.0003    0.000    0.001    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, - Z
SFAC  C    H    O    SN   CL
UNIT  12   28   4    4    4
MERG   2
FMAP   2
PLAN   20
ACTA
BOND   $H
CONF
LIST   4
WPDB  -2
L.S.   4
TEMP  -123.00
WGHT    0.041000    0.543500
FVAR       0.59355
SN1   4    0.804090    0.101536    0.530161    11.00000    0.02057    0.01826 =
         0.01798   -0.00033    0.00698    0.00273
CL    5    0.666475   -0.077489    0.668773    11.00000    0.01966    0.03292 =
         0.02466    0.00718    0.00953    0.00116
O1    3    0.881435   -0.028388    0.372061    11.00000    0.01579    0.02525 =
         0.01511   -0.00092    0.00540    0.00153
C2    1    0.763189   -0.042575    0.214809    11.00000    0.01750    0.02068 =
         0.01821   -0.00160    0.00532   -0.00296
AFIX  13
H2    2    0.618582   -0.070063    0.213794    11.00000   -1.20000
AFIX   0
C3    1    0.860107   -0.147992    0.137541    11.00000    0.02633    0.02913 =
         0.02241   -0.00691    0.00361    0.00212
AFIX 137
H3A   2    1.000329   -0.121184    0.134264    11.00000   -1.50000
H3B   2    0.774359   -0.161314    0.033478    11.00000   -1.50000
H3C   2    0.868126   -0.229453    0.195056    11.00000   -1.50000
AFIX   0
C4    1    0.751655    0.086006    0.132679    11.00000    0.02735    0.02924 =
         0.02085    0.00531    0.00343   -0.00062
AFIX 137
H4A   2    0.680666    0.150127    0.181575    11.00000   -1.50000
H4B   2    0.674147    0.074847    0.026039    11.00000   -1.50000
H4C   2    0.892657    0.116596    0.137054    11.00000   -1.50000
HKLF    4

REM  import in P 21/a
REM R1 =  0.0282 for   1310 Fo > 4sig(Fo)  and  0.0295 for all   1368 data
REM     57 parameters refined using      0 restraints

END

WGHT      0.0411      0.5357
 REM Highest difference peak   0.85,  deepest hole  -1.47,  1-sigma level   0.18
Q1    1   0.8752  0.1018  0.3577  11.00000  0.05    0.85
Q2    1   0.8725  0.0323  0.4248  11.00000  0.05    0.83
Q3    1   0.7534  0.1012  0.6881  11.00000  0.05    0.74
Q4    1   0.8560  0.1483  0.6071  11.00000  0.05    0.69
Q5    1   0.7764  0.1593  0.6150  11.00000  0.05    0.65
Q6    1   0.6577  0.0138  0.6634  11.00000  0.05    0.65
Q7    1   0.8421 -0.3174  0.3396  11.00000  0.05    0.63
Q8    1   0.7465  0.0367  0.6344  11.00000  0.05    0.62
Q9    1   0.9123  0.1760  0.4224  11.00000  0.05    0.57
Q10   1   0.7701  0.1451  0.4479  11.00000  0.05    0.52
Q11   1   1.0963  0.0229  0.3533  11.00000  0.05    0.52
Q12   1   0.7485  0.0042  0.1615  11.00000  0.05    0.50
Q13   1   0.7279  0.1144  0.4450  11.00000  0.05    0.48
Q14   1   0.6458  0.0168  0.4822  11.00000  0.05    0.47
Q15   1   0.8196 -0.4023  0.2435  11.00000  0.05    0.45
Q16   1   0.7273  0.2386  0.4233  11.00000  0.05    0.45
Q17   1   1.0440 -0.0984  0.2780  11.00000  0.05    0.44
Q18   1   1.0201 -0.0345  0.1582  11.00000  0.05    0.43
Q19   1   0.5152  0.0214  0.6389  11.00000  0.05    0.42
Q20   1   0.8089  0.0165  0.3004  11.00000  0.05    0.42
;
_cod_data_source_file            om5007566_si_001.cif
_cod_data_source_block           {Sn(OiPr}{Cl}}2
_cod_depositor_comments
'Adding full bibliography for 4084635--4084638.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4084638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.80409(3) 0.10154(2) 0.53016(2) 0.01856(12) Uani 1 1 d .
Cl Cl 0.66647(13) -0.07749(9) 0.66877(11) 0.0250(2) Uani 1 1 d .
O1 O 0.8814(3) -0.0284(2) 0.3721(3) 0.0185(5) Uani 1 1 d .
C2 C 0.7632(5) -0.0426(3) 0.2148(4) 0.0187(6) Uani 1 1 d .
H2 H 0.6186 -0.0701 0.2138 0.022 Uiso 1 1 calc R
C3 C 0.8601(5) -0.1480(4) 0.1375(4) 0.0264(7) Uani 1 1 d .
H3A H 1.0003 -0.1212 0.1343 0.04 Uiso 1 1 calc R
H3B H 0.7744 -0.1613 0.0335 0.04 Uiso 1 1 calc R
H3C H 0.8681 -0.2295 0.1951 0.04 Uiso 1 1 calc R
C4 C 0.7517(6) 0.0860(3) 0.1327(5) 0.0263(8) Uani 1 1 d .
H4A H 0.6807 0.1501 0.1816 0.039 Uiso 1 1 calc R
H4B H 0.6741 0.0748 0.026 0.039 Uiso 1 1 calc R
H4C H 0.8927 0.1166 0.1371 0.039 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.02057(16) 0.01826(18) 0.01798(18) -0.00033(8) 0.00698(11) 0.00273(7)
Cl 0.0197(4) 0.0329(5) 0.0247(5) 0.0072(4) 0.0095(3) 0.0012(3)
O1 0.0158(10) 0.0252(12) 0.0151(11) -0.0009(10) 0.0054(8) 0.0015(9)
C2 0.0175(14) 0.0207(17) 0.0182(16) -0.0016(13) 0.0053(12) -0.0030(11)
C3 0.0263(17) 0.029(2) 0.0224(18) -0.0069(16) 0.0036(14) 0.0021(15)
C4 0.0273(19) 0.029(2) 0.0208(18) 0.0053(14) 0.0034(15) -0.0006(13)
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Sn1 O1 71.67(10) . 3_756
O1 Sn1 Cl 93.51(7) . .
O1 Sn1 Cl 88.79(6) 3_756 .
C2 O1 Sn1 124.48(18) . .
C2 O1 Sn1 125.93(18) . 3_756
Sn1 O1 Sn1 108.33(10) . 3_756
O1 C2 C4 110.2(3) . .
O1 C2 C3 109.8(3) . .
C4 C2 C3 111.6(3) . .
O1 C2 H2 108.4 . .
C4 C2 H2 108.4 . .
C3 C2 H2 108.4 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O1 2.117(2) .
Sn1 O1 2.185(2) 3_756
Sn1 Cl 2.5273(9) .
O1 C2 1.450(4) .
C2 C4 1.508(5) .
C2 C3 1.520(5) .
C2 H2 1 .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C4 H4A 0.98 .
C4 H4B 0.98 .
C4 H4C 0.98 .
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_4
O1 Sn1 O1 C2 -167.8(3) 3_756 .
Cl Sn1 O1 C2 104.7(2) . .
O1 Sn1 O1 Sn1 0 3_756 3_756
Cl Sn1 O1 Sn1 -87.55(9) . 3_756
Sn1 O1 C2 C4 58.7(3) . .
Sn1 O1 C2 C4 -106.9(3) 3_756 .
Sn1 O1 C2 C3 -177.9(2) . .
Sn1 O1 C2 C3 16.4(4) 3_756 .
