#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/70/2237060.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_2237060
loop_
_publ_author_name
'Sow, Yaya'
'Diop, Libasse'
'Molloy, Kieran C.'
'Kociok-Köhn, Gabriele'
_publ_section_title
;
 Di-μ-hydroxido-bis[dimethyl(thiocyanato-κN)tin(IV)]
;
_journal_coeditor_code           WM2689
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1436
_journal_paper_doi               10.1107/S1600536812043462
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Sn2 (C H3)4 (N C S)2 (O H)2]'
_chemical_formula_moiety         'C6 H14 N2 O2 S2 Sn2'
_chemical_formula_sum            'C6 H14 N2 O2 S2 Sn2'
_chemical_formula_weight         447.69
_chemical_name_systematic
;
Di-μ-hydroxido-bis[dimethyl(thiocyanato-κN)tin(IV)]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3440(2)
_cell_length_b                   12.5214(3)
_cell_length_c                   13.3871(2)
_cell_measurement_reflns_used    30989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1398.66(5)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '584 1.0 degree images with 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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20098
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  0.6994
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.643
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1603
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+1.8745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                1333
_reflns_number_total             1603
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2689.cif
_cod_data_source_block           I
_cod_original_cell_volume        1398.67(5)
_cod_database_code               2237060
_cod_database_fobs_code          2237060
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'
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 Sn 0.20586(3) 0.512859(18) 0.486833(17) 0.02446(10) Uani d . 1 1
S S 0.55735(12) 0.27972(7) 0.69604(7) 0.0356(2) Uani d . 1 1
O O 0.0319(3) 0.4300(2) 0.5594(2) 0.0365(6) Uani d D 1 1
N N 0.3739(3) 0.4101(2) 0.5723(2) 0.0301(6) Uani d . 1 1
C C1 0.2597(4) 0.4461(3) 0.3467(3) 0.0337(8) Uani d . 1 1
H H1A 0.1938 0.3823 0.3361 0.051 Uiso calc R 1 1
H H1B 0.3733 0.4264 0.3445 0.051 Uiso calc R 1 1
H H1C 0.2371 0.4985 0.2942 0.051 Uiso calc R 1 1
C C2 0.2640(4) 0.6541(3) 0.5634(3) 0.0326(8) Uani d . 1 1
H H2A 0.2317 0.7159 0.5233 0.049 Uiso calc R 1 1
H H2B 0.3799 0.6566 0.5751 0.049 Uiso calc R 1 1
H H2C 0.2076 0.6556 0.6276 0.049 Uiso calc R 1 1
C C3 0.4481(4) 0.3549(3) 0.6243(2) 0.0247(7) Uani d . 1 1
H H10 0.054(4) 0.377(2) 0.596(2) 0.033(10) Uiso d D 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn 0.01938(14) 0.02506(15) 0.02894(15) 0.00034(9) -0.00069(9) 0.00358(8)
S 0.0431(5) 0.0317(5) 0.0319(5) 0.0115(4) -0.0139(4) -0.0056(3)
O 0.0234(13) 0.0358(15) 0.0501(16) 0.0009(11) -0.0028(12) 0.0229(12)
N 0.0249(15) 0.0311(16) 0.0342(16) 0.0036(13) -0.0038(13) 0.0023(12)
C1 0.032(2) 0.034(2) 0.036(2) -0.0050(16) -0.0056(15) -0.0037(15)
C2 0.034(2) 0.033(2) 0.0311(19) 0.0002(15) 0.0040(15) -0.0044(15)
C3 0.0200(17) 0.0275(18) 0.0266(16) -0.0032(14) 0.0030(14) -0.0071(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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O Sn C2 . . 111.20(13)
O Sn C1 . . 112.11(13)
C2 Sn C1 . . 136.11(15)
O Sn O . 5_566 69.90(10)
C2 Sn O . 5_566 94.13(12)
C1 Sn O . 5_566 94.06(13)
O Sn N . . 84.76(10)
C2 Sn N . . 95.18(12)
C1 Sn N . . 95.43(13)
O Sn N 5_566 . 154.66(10)
Sn O Sn . 5_566 110.10(10)
Sn O H10 . . 122(3)
Sn O H10 5_566 . 128(3)
C3 N Sn . . 172.5(3)
Sn C1 H1A . . 109.5
Sn C1 H1B . . 109.5
H1A C1 H1B . . 109.5
Sn C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
Sn C2 H2A . . 109.5
Sn C2 H2B . . 109.5
H2A C2 H2B . . 109.5
Sn C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
N C3 S . . 178.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn O . 2.032(2)
Sn C2 . 2.101(4)
Sn C1 . 2.102(4)
Sn O 5_566 2.198(2)
Sn N . 2.220(3)
S C3 . 1.625(4)
O Sn 5_566 2.198(2)
O H10 . 0.842(18)
N C3 . 1.160(4)
C1 H1A . 0.9800
C1 H1B . 0.9800
C1 H1C . 0.9800
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 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
O H10 S 8_565 0.842(18) 2.38(2) 3.207(3) 168(4)
C2 H2C S 3_466 0.98 2.79 3.746(4) 164.2
