#------------------------------------------------------------------------------
#$Date: 2016-10-01 04:41:17 +0300 (Sat, 01 Oct 2016) $
#$Revision: 186858 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/18/2241865.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_2241865
loop_
_publ_author_name
'Otte, Felix'
'Koller, Stephan G.'
'Golz, Christopher'
'Strohmann, Carsten'
_publ_section_title
;
 Crystal structures of diaquadi-μ-hydroxido-tris[trimethyltin(IV)]
 diformatotrimethylstannate(IV) and di-μ-hydroxido-tris[trimethyltin(IV)]
 chloride monohydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1499
_journal_page_last               1502
_journal_paper_doi               10.1107/S2056989016014912
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Sn3 (C H3)9 (O H)2] Cl, H2 O'
_chemical_formula_moiety         'C9 H29 O2 Sn3 +, Cl -, H2 O'
_chemical_formula_sum            'C9 H31 Cl O3 Sn3'
_chemical_formula_weight         578.86
_chemical_name_systematic
;
Di-μ-hydroxido-tris[trimethyltin(IV)] chloride monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.623(3)
_cell_length_b                   8.2675(18)
_cell_length_c                   18.421(5)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.94
_cell_volume                     1922.4(8)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX3 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16017
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.686
_diffrn_reflns_theta_min         2.211
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.001
_exptl_absorpt_correction_T_max  0.0320
_exptl_absorpt_correction_T_min  0.0103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.383
_refine_ls_abs_structure_details
;
Flack x determined using 2271 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.026(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0269P)²+0.6817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                5072
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            su5326sup1.cif
_cod_data_source_block           2
_cod_database_code               2241865
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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_occupancy
C C1 0.7513(5) 0.1853(7) 0.7655(3) 0.0397(11) Uani d 1
H H1A 0.7352 0.2995 0.7566 0.059 Uiso calc 1
H H1B 0.8181 0.1767 0.7924 0.059 Uiso calc 1
H H1C 0.6941 0.1366 0.7941 0.059 Uiso calc 1
C C2 0.7054(4) -0.1756(6) 0.6542(3) 0.0345(10) Uani d 1
H H2A 0.6448 -0.1902 0.6868 0.052 Uiso calc 1
H H2B 0.7609 -0.2537 0.6667 0.052 Uiso calc 1
H H2C 0.6828 -0.1931 0.6039 0.052 Uiso calc 1
C C3 0.8814(4) 0.1523(7) 0.5927(3) 0.0358(11) Uani d 1
H H3A 0.8661 0.1136 0.5435 0.054 Uiso calc 1
H H3B 0.9515 0.1141 0.6077 0.054 Uiso calc 1
H H3C 0.8802 0.2709 0.5933 0.054 Uiso calc 1
C C4 0.6887(5) 0.4752(7) 0.5271(3) 0.0436(13) Uani d 1
H H4A 0.7587 0.4640 0.5046 0.065 Uiso calc 1
H H4B 0.6969 0.4882 0.5797 0.065 Uiso calc 1
H H4C 0.6527 0.5702 0.5071 0.065 Uiso calc 1
C C5 0.4333(5) 0.2706(8) 0.5290(3) 0.0490(15) Uani d 1
H H5A 0.4053 0.3790 0.5191 0.073 Uiso calc 1
H H5B 0.4221 0.2438 0.5802 0.073 Uiso calc 1
H H5C 0.3965 0.1915 0.4984 0.073 Uiso calc 1
C C6 0.6638(5) 0.0545(6) 0.4578(3) 0.0381(11) Uani d 1
H H6A 0.6173 0.0158 0.4189 0.057 Uiso calc 1
H H6B 0.6712 -0.0298 0.4948 0.057 Uiso calc 1
H H6C 0.7336 0.0803 0.4376 0.057 Uiso calc 1
C C7 0.7215(4) 0.6488(6) 0.3435(3) 0.0367(10) Uani d 1
H H7A 0.7630 0.5597 0.3640 0.055 Uiso calc 1
H H7B 0.7275 0.7439 0.3750 0.055 Uiso calc 1
H H7C 0.7485 0.6753 0.2950 0.055 Uiso calc 1
C C8 0.4542(4) 0.7036(6) 0.4051(3) 0.0359(11) Uani d 1
H H8A 0.3839 0.6535 0.4026 0.054 Uiso calc 1
H H8B 0.4493 0.8169 0.3898 0.054 Uiso calc 1
H H8C 0.4806 0.6985 0.4551 0.054 Uiso calc 1
C C9 0.5063(5) 0.4823(7) 0.2352(3) 0.0390(11) Uani d 1
H H9A 0.5524 0.5207 0.1960 0.059 Uiso calc 1
H H9B 0.4335 0.5179 0.2260 0.059 Uiso calc 1
H H9C 0.5085 0.3639 0.2371 0.059 Uiso calc 1
O O1 0.6340(3) 0.1729(4) 0.61594(19) 0.0327(7) Uani d 1
H H1 0.575(4) 0.168(9) 0.648(3) 0.06(2) Uiso d 1
O O2 0.5652(3) 0.3638(4) 0.39350(19) 0.0333(7) Uani d 1
H H2 0.519(4) 0.293(6) 0.369(3) 0.040(16) Uiso d 1
Sn Sn1 0.76540(2) 0.06256(3) 0.66540(2) 0.02692(7) Uani d 1
Sn Sn2 0.59742(2) 0.26536(3) 0.50553(2) 0.02755(7) Uani d 1
Sn Sn3 0.55935(2) 0.57842(4) 0.33566(2) 0.02786(7) Uani d 1
O O3 0.4394(3) 0.1219(5) 0.3417(3) 0.0488(10) Uani d 1
H H3D 0.467(7) 0.043(8) 0.308(4) 0.08(3) Uiso d 1
H H3E 0.365(4) 0.127(15) 0.328(10) 0.18(6) Uiso d 1
Cl Cl1 0.94986(10) -0.10984(17) 0.73601(7) 0.0379(3) Uani d 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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_3
_geom_angle
H1A C1 H1B . 109.5
H1A C1 H1C . 109.5
H1B C1 H1C . 109.5
Sn1 C1 H1A . 109.5
Sn1 C1 H1B . 109.5
Sn1 C1 H1C . 109.5
H2A C2 H2B . 109.5
H2A C2 H2C . 109.5
H2B C2 H2C . 109.5
Sn1 C2 H2A . 109.5
Sn1 C2 H2B . 109.5
Sn1 C2 H2C . 109.5
H3A C3 H3B . 109.5
H3A C3 H3C . 109.5
H3B C3 H3C . 109.5
Sn1 C3 H3A . 109.5
Sn1 C3 H3B . 109.5
Sn1 C3 H3C . 109.5
H4A C4 H4B . 109.5
H4A C4 H4C . 109.5
H4B C4 H4C . 109.5
Sn2 C4 H4A . 109.5
Sn2 C4 H4B . 109.5
Sn2 C4 H4C . 109.5
H5A C5 H5B . 109.5
H5A C5 H5C . 109.5
H5B C5 H5C . 109.5
Sn2 C5 H5A . 109.5
Sn2 C5 H5B . 109.5
Sn2 C5 H5C . 109.5
H6A C6 H6B . 109.5
H6A C6 H6C . 109.5
H6B C6 H6C . 109.5
Sn2 C6 H6A . 109.5
Sn2 C6 H6B . 109.5
Sn2 C6 H6C . 109.5
H7A C7 H7B . 109.5
H7A C7 H7C . 109.5
H7B C7 H7C . 109.5
Sn3 C7 H7A . 109.5
Sn3 C7 H7B . 109.5
Sn3 C7 H7C . 109.5
H8A C8 H8B . 109.5
H8A C8 H8C . 109.5
H8B C8 H8C . 109.5
Sn3 C8 H8A . 109.5
Sn3 C8 H8B . 109.5
Sn3 C8 H8C . 109.5
H9A C9 H9B . 109.5
H9A C9 H9C . 109.5
H9B C9 H9C . 109.5
Sn3 C9 H9A . 109.5
Sn3 C9 H9B . 109.5
Sn3 C9 H9C . 109.5
Sn1 O1 H1 . 109(4)
Sn1 O1 Sn2 . 135.30(17)
Sn2 O1 H1 . 115(4)
Sn2 O2 H2 . 109(4)
Sn3 O2 H2 . 105(4)
Sn3 O2 Sn2 . 141.84(17)
C1 Sn1 C2 . 120.1(2)
C1 Sn1 C3 . 116.2(2)
C1 Sn1 Cl1 . 85.16(17)
C2 Sn1 Cl1 . 83.06(14)
C3 Sn1 C2 . 120.7(2)
C3 Sn1 Cl1 . 84.55(15)
O1 Sn1 C1 . 95.96(19)
O1 Sn1 C2 . 94.52(17)
O1 Sn1 C3 . 96.85(17)
O1 Sn1 Cl1 . 177.58(10)
C4 Sn2 C6 . 122.3(3)
C4 Sn2 O1 . 89.81(18)
C4 Sn2 O2 . 88.55(17)
C5 Sn2 C4 . 118.5(3)
C5 Sn2 C6 . 119.2(3)
C5 Sn2 O1 . 91.36(18)
C5 Sn2 O2 . 90.15(19)
C6 Sn2 O1 . 90.83(17)
C6 Sn2 O2 . 89.35(17)
O1 Sn2 O2 . 178.17(14)
C8 Sn3 C7 . 115.3(2)
C8 Sn3 C9 . 120.9(2)
C9 Sn3 C7 . 117.6(2)
O2 Sn3 C7 . 99.50(18)
O2 Sn3 C8 . 97.50(17)
O2 Sn3 C9 . 97.99(18)
H3D O3 H3E . 102(10)
Sn1 Cl1 Sn3 4_645 127.21(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 H1A . 0.9800
C1 H1B . 0.9800
C1 H1C . 0.9800
C1 Sn1 . 2.113(5)
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C2 Sn1 . 2.120(5)
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
C3 Sn1 . 2.118(5)
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C4 Sn2 . 2.120(5)
C5 H5A . 0.9800
C5 H5B . 0.9800
C5 H5C . 0.9800
C5 Sn2 . 2.117(6)
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
C6 Sn2 . 2.125(5)
C7 H7A . 0.9800
C7 H7B . 0.9800
C7 H7C . 0.9800
C7 Sn3 . 2.133(5)
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C8 Sn3 . 2.114(5)
C9 H9A . 0.9800
C9 H9B . 0.9800
C9 H9C . 0.9800
C9 Sn3 . 2.123(5)
O1 H1 . 0.95(3)
O1 Sn1 . 2.100(3)
O1 Sn2 . 2.222(3)
O2 H2 . 0.94(3)
O2 Sn2 . 2.255(4)
O2 Sn3 . 2.071(3)
Sn1 Cl1 . 3.0240(14)
O3 H3D . 0.97(3)
O3 H3E . 0.98(3)
Cl1 Sn3 4_645 3.1663(15)
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
O2 H2 O3 . 0.94(3) 1.81(3) 2.726(5) 164(6)
O1 H1 Cl1 3_455 0.95(3) 2.32(3) 3.251(4) 168(6)
O3 H3D Cl1 4_654 0.97(3) 2.10(3) 3.068(5) 171(8)

_cod_database_fobs_code 2241865
