#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/44/2234453.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_2234453
loop_
_publ_author_name
'Amini, Mostafa M.'
'Ng, Seik Weng'
_publ_section_title
;
 Di-μ-chlorido-bis[aquachloridodimethyltin(IV)]--1,4,7,10,13-pentaoxacyclopentadecane
 (1/1)
;
_journal_coeditor_code           XU5444
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m354
_journal_paper_doi               10.1107/S1600536812008781
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Sn2 (C H3)4 Cl4 (H2 O)2], C10 H20 O5'
_chemical_formula_moiety         'C4 H16 Cl4 O2 Sn2, C10 H20 O5'
_chemical_formula_sum            'C14 H36 Cl4 O7 Sn2'
_chemical_formula_weight         695.61
_chemical_name_systematic
;
Di-μ-chlorido-bis[aquachloridodimethyltin(IV)]--1,4,7,10,13-
pentaoxacyclopentadecane (1/1)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 127.183(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2351(13)
_cell_length_b                   11.4115(5)
_cell_length_c                   9.8100(9)
_cell_measurement_reflns_used    5314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4898
_cell_measurement_theta_min      2.5269
_cell_volume                     1269.6(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5824
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_T_max  0.6435
_exptl_absorpt_correction_T_min  0.5309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.716
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1524
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0230P)²+2.1038P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0418
_reflns_number_gt                1495
_reflns_number_total             1524
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu5444.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2234453
_cod_database_fobs_code          2234453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn Sn1 0.655960(17) 0.5000 0.51206(2) 0.01800(8) Uani d S 1 2 . .
Cl Cl1 0.43822(7) 0.5000 0.25799(9) 0.02629(17) Uani d S 1 2 . .
Cl Cl2 0.73232(8) 0.5000 0.35183(10) 0.02918(17) Uani d S 1 2 . .
O O1W 0.8420(2) 0.5000 0.7676(3) 0.0329(5) Uani d S 1 2 . .
H H1 0.8512 0.5605 0.8232 0.049 Uiso calc RD 1 1 . .
O O1 0.8868(4) 0.5018(14) 1.0827(5) 0.0187(5) Uani d SPDU 0.25 1 A -1
O O2 1.0086(8) 0.6816(7) 1.0770(10) 0.0187(5) Uani d PD 0.25 1 A -1
O O3 1.0110(5) 0.6179(5) 0.7954(7) 0.0187(5) Uani d PD 0.25 1 A -1
O O4 1.0459(5) 0.3741(5) 0.8555(7) 0.0187(5) Uani d PD 0.25 1 A -1
O O5 1.0106(8) 0.3021(7) 1.1028(10) 0.0187(5) Uani d PD 0.25 1 A -1
C C1 0.8963(15) 0.6095(12) 1.164(2) 0.0199(5) Uani d PDU 0.25 1 A -1
H H1A 0.9664 0.6078 1.2858 0.024 Uiso calc PR 0.25 1 A -1
H H1B 0.8255 0.6215 1.1595 0.024 Uiso calc PR 0.25 1 A -1
C C2 0.9075(17) 0.7073(16) 1.072(3) 0.0199(5) Uani d PD 0.25 1 A -1
H H2A 0.8355 0.7121 0.9520 0.024 Uiso calc PR 0.25 1 A -1
H H2B 0.9183 0.7831 1.1288 0.024 Uiso calc PR 0.25 1 A -1
C C3 1.0255(10) 0.7633(8) 0.9801(15) 0.0199(5) Uani d PD 0.25 1 A -1
H H3A 1.0707 0.8324 1.0511 0.024 Uiso calc PR 0.25 1 A -1
H H3B 0.9482 0.7904 0.8774 0.024 Uiso calc PR 0.25 1 A -1
C C4 1.0921(13) 0.7001(12) 0.928(2) 0.0199(5) Uani d PD 0.25 1 A -1
H H4A 1.1211 0.7565 0.8846 0.024 Uiso calc PR 0.25 1 A -1
H H4B 1.1606 0.6582 1.0273 0.024 Uiso calc PR 0.25 1 A -1
C C5 1.0639(7) 0.5468(6) 0.7385(10) 0.0199(5) Uani d PD 0.25 1 A -1
H H5A 1.1192 0.5954 0.7333 0.024 Uiso calc PR 0.25 1 A -1
H H5B 1.0017 0.5182 0.6215 0.024 Uiso calc PR 0.25 1 A -1
C C6 1.1287(7) 0.4445(6) 0.8525(11) 0.0199(5) Uani d PD 0.25 1 A -1
H H6A 1.1640 0.3978 0.8088 0.024 Uiso calc PR 0.25 1 A -1
H H6B 1.1929 0.4717 0.9695 0.024 Uiso calc PR 0.25 1 A -1
C C7 1.0979(8) 0.2730(8) 0.9620(13) 0.0199(5) Uani d PD 0.25 1 A -1
H H7A 1.1728 0.2947 1.0729 0.024 Uiso calc PR 0.25 1 A -1
H H7B 1.1153 0.2138 0.9063 0.024 Uiso calc PR 0.25 1 A -1
C C8 1.0136(11) 0.2234(7) 0.9908(17) 0.0199(5) Uani d PD 0.25 1 A -1
H H8A 0.9339 0.2159 0.8806 0.024 Uiso calc PR 0.25 1 A -1
H H8B 1.0402 0.1447 1.0436 0.024 Uiso calc PR 0.25 1 A -1
C C9 0.9022(14) 0.2965(13) 1.084(3) 0.0199(5) Uani d PD 0.25 1 A -1
H H9A 0.8978 0.2221 1.1316 0.024 Uiso calc PR 0.25 1 A -1
H H9B 0.8338 0.3004 0.9611 0.024 Uiso calc PR 0.25 1 A -1
C C10 0.9009(15) 0.3995(12) 1.179(2) 0.0199(5) Uani d PD 0.25 1 A -1
H H10A 0.8346 0.3926 1.1861 0.024 Uiso calc PR 0.25 1 A -1
H H10B 0.9756 0.4036 1.2963 0.024 Uiso calc PR 0.25 1 A -1
C C11 0.6536(2) 0.68104(19) 0.5528(3) 0.0271(5) Uani d . 1 1 . .
H H11 0.6202 0.6940 0.6144 0.041 Uiso calc R 1 1 . .
H H12 0.6053 0.7215 0.4423 0.041 Uiso calc R 1 1 . .
H H13 0.7343 0.7118 0.6206 0.041 Uiso calc R 1 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'
O O 0.0106 0.0060 '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'
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
C11 Sn1 C11 . 6_565 157.00(13)
C11 Sn1 O1W . . 86.16(7)
C11 Sn1 O1W 6_565 . 86.16(7)
C11 Sn1 Cl2 . . 100.96(6)
C11 Sn1 Cl2 6_565 . 100.96(6)
O1W Sn1 Cl2 . . 92.01(7)
C11 Sn1 Cl1 . . 92.07(7)
C11 Sn1 Cl1 6_565 . 92.07(7)
O1W Sn1 Cl1 . . 170.83(7)
Cl2 Sn1 Cl1 . . 97.16(3)
C11 Sn1 Cl1 . 5_666 78.93(6)
C11 Sn1 Cl1 6_565 5_666 78.93(6)
O1W Sn1 Cl1 . 5_666 85.96(7)
Cl2 Sn1 Cl1 . 5_666 177.97(3)
Cl1 Sn1 Cl1 . 5_666 84.87(3)
Sn1 O1W H1 . . 109.5
C1 O1 C10 . . 113.8(4)
C2 O2 C3 . . 113.8(7)
C5 O3 C4 . . 113.4(6)
C7 O4 C6 . . 113.4(6)
C8 O5 C9 . . 113.4(8)
O1 C1 C2 . . 108.1(8)
O1 C1 H1A . . 110.1
C2 C1 H1A . . 110.1
O1 C1 H1B . . 110.1
C2 C1 H1B . . 110.1
H1A C1 H1B . . 108.4
O2 C2 C1 . . 107.1(8)
O2 C2 H2A . . 110.3
C1 C2 H2A . . 110.3
O2 C2 H2B . . 110.3
C1 C2 H2B . . 110.3
H2A C2 H2B . . 108.5
O2 C3 C4 . . 107.6(8)
O2 C3 H3A . . 110.2
C4 C3 H3A . . 110.2
O2 C3 H3B . . 110.2
C4 C3 H3B . . 110.2
H3A C3 H3B . . 108.5
O3 C4 C3 . . 107.0(9)
O3 C4 H4A . . 110.3
C3 C4 H4A . . 110.3
O3 C4 H4B . . 110.3
C3 C4 H4B . . 110.3
H4A C4 H4B . . 108.6
O3 C5 C6 . . 112.7(5)
O3 C5 H5A . . 109.1
C6 C5 H5A . . 109.1
O3 C5 H5B . . 109.1
C6 C5 H5B . . 109.1
H5A C5 H5B . . 107.8
O4 C6 C5 . . 108.0(6)
O4 C6 H6A . . 110.1
C5 C6 H6A . . 110.1
O4 C6 H6B . . 110.1
C5 C6 H6B . . 110.1
H6A C6 H6B . . 108.4
O4 C7 C8 . . 108.9(7)
O4 C7 H7A . . 109.9
C8 C7 H7A . . 109.9
O4 C7 H7B . . 109.9
C8 C7 H7B . . 109.9
H7A C7 H7B . . 108.3
O5 C8 C7 . . 107.7(7)
O5 C8 H8A . . 110.2
C7 C8 H8A . . 110.2
O5 C8 H8B . . 110.2
C7 C8 H8B . . 110.2
H8A C8 H8B . . 108.5
O5 C9 C10 . . 107.4(8)
O5 C9 H9A . . 110.2
C10 C9 H9A . . 110.2
O5 C9 H9B . . 110.2
C10 C9 H9B . . 110.2
H9A C9 H9B . . 108.5
O1 C10 C9 . . 106.0(8)
O1 C10 H10A . . 110.5
C9 C10 H10A . . 110.5
O1 C10 H10B . . 110.5
C9 C10 H10B . . 110.5
H10A C10 H10B . . 108.7
Sn1 C11 H11 . . 109.5
Sn1 C11 H12 . . 109.5
H11 C11 H12 . . 109.5
Sn1 C11 H13 . . 109.5
H11 C11 H13 . . 109.5
H12 C11 H13 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn1 C11 . 2.108(2)
Sn1 C11 6_565 2.108(2)
Sn1 O1W . 2.296(2)
Sn1 Cl2 . 2.3912(8)
Sn1 Cl1 . 2.5459(10)
Sn1 Cl1 5_666 3.2467(9)
O1W H1 . 0.8400
O1 C1 . 1.427(9)
O1 C10 . 1.438(9)
O2 C2 . 1.440(10)
O2 C3 . 1.452(8)
O3 C5 . 1.430(7)
O3 C4 . 1.447(10)
O4 C7 . 1.427(8)
O4 C6 . 1.442(7)
O5 C8 . 1.439(8)
O5 C9 . 1.439(9)
C1 C2 . 1.505(9)
C1 H1A . 0.9900
C1 H1B . 0.9900
C2 H2A . 0.9900
C2 H2B . 0.9900
C3 C4 . 1.504(9)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 H4A . 0.9900
C4 H4B . 0.9900
C5 C6 . 1.489(8)
C5 H5A . 0.9900
C5 H5B . 0.9900
C6 H6A . 0.9900
C6 H6B . 0.9900
C7 C8 . 1.501(8)
C7 H7A . 0.9900
C7 H7B . 0.9900
C8 H8A . 0.9900
C8 H8B . 0.9900
C9 C10 . 1.508(9)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 H11 . 0.9800
C11 H12 . 0.9800
C11 H13 . 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
O1w H1 O1 . 0.84 2.37 2.753(4) 108
O1w H1 O1 6_565 0.84 2.38 2.753(4) 107
O1w H1 O2 2_757 0.84 2.12 2.687(9) 125
O1w H1 O5 5_767 0.84 2.26 2.810(9) 123
