#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324418.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_4324418
loop_
_publ_author_name
'Ravi Shankar'
'Archana Jain'
'Gabriele Kociok-Köhn'
'Kieran C. Molloy'
_publ_section_title
;
 Diorganotin-Based Coordination Polymers Derived from
 Sulfonate/Phosphonate/Phosphonocarboxylate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1339
_journal_page_last               1350
_journal_paper_doi               10.1021/ic1018423
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H32 O16 P2 S2 Sn3'
_chemical_formula_sum            'C16 H32 O16 P2 S2 Sn3'
_chemical_formula_weight         962.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           91
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w 2c'
_symmetry_space_group_name_H-M   'P 41 2 2'
_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                   10.61360(10)
_cell_length_b                   10.61360(10)
_cell_length_c                   28.72110(10)
_cell_measurement_reflns_used    44128
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     3235.39(4)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). 
 Sheldrick, G.M., Institüt für Anorganische Chemie der Universität, 
 Tammanstrasse 4, D-3400 Göttingen, Germany, 1998 
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '451 1.5 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  0.1679
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            46641
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.589
_exptl_absorpt_correction_T_max  0.6251
_exptl_absorpt_correction_T_min  0.5633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.790
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+2.7347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                4081
_reflns_number_total             4736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1018423_si_001_5.cif
_cod_data_source_block           compound5
_cod_original_sg_symbol_H-M      ' P 41 2 2'
_cod_database_code               4324418
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z+1/2'
'-x, y, -z'
'-y, -x, -z+1/4'
'y, x, -z+3/4'
'y, -x, z+3/4'
'-y, x, z+1/4'
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 0.68207(3) 0.12470(3) 0.055073(12) 0.02113(9) Uani 1 1 d .
Sn2 Sn 1.04854(3) -0.04854(3) 0.1250 0.01802(11) Uani 1 2 d S
P P 0.96126(12) 0.23764(12) 0.08812(4) 0.0182(2) Uani 1 1 d .
S S 0.90903(13) -0.35105(12) 0.16817(5) 0.0262(3) Uani 1 1 d .
O1 O 0.8742(3) 0.1704(3) 0.05403(12) 0.0227(7) Uani 1 1 d .
O2 O 0.8857(3) 0.3158(3) 0.12337(12) 0.0221(7) Uani 1 1 d .
O3 O 1.0481(3) 0.1450(3) 0.11334(12) 0.0210(7) Uani 1 1 d .
O4 O 1.1944(6) 0.5444(6) 0.01553(17) 0.0689(17) Uani 1 1 d .
O5 O 1.3119(5) 0.5669(5) 0.07898(18) 0.0651(16) Uani 1 1 d .
O6 O 1.0159(4) -0.2750(3) 0.15275(13) 0.0290(8) Uani 1 1 d .
O7 O 0.9539(4) -0.4772(3) 0.18125(15) 0.0342(9) Uani 1 1 d .
O8 O 0.8323(4) -0.2950(4) 0.20440(14) 0.0360(10) Uani 1 1 d .
C1 C 0.6184(6) 0.3088(5) 0.0475(2) 0.0318(12) Uani 1 1 d .
H1A H 0.5273 0.3083 0.0419 0.048 Uiso 1 1 calc R
H1B H 0.6613 0.3484 0.0211 0.048 Uiso 1 1 calc R
H1C H 0.6364 0.3564 0.0759 0.048 Uiso 1 1 calc R
C2 C 0.7004(5) -0.0582(5) 0.02934(18) 0.0265(11) Uani 1 1 d .
H2A H 0.6928 -0.1185 0.0550 0.040 Uiso 1 1 calc R
H2B H 0.7830 -0.0677 0.0145 0.040 Uiso 1 1 calc R
H2C H 0.6339 -0.0743 0.0064 0.040 Uiso 1 1 calc R
C3 C 1.0532(5) 0.3479(5) 0.05536(18) 0.0239(10) Uani 1 1 d .
H3A H 1.1012 0.3014 0.0314 0.029 Uiso 1 1 calc R
H3B H 0.9953 0.4063 0.0390 0.029 Uiso 1 1 calc R
C4 C 1.1447(5) 0.4248(5) 0.08436(19) 0.0296(12) Uani 1 1 d .
H4A H 1.0975 0.4708 0.1087 0.036 Uiso 1 1 calc R
H4B H 1.2045 0.3672 0.1001 0.036 Uiso 1 1 calc R
C5 C 1.2174(6) 0.5175(5) 0.0553(2) 0.0358(13) Uani 1 1 d .
C6 C 1.3866(9) 0.6635(9) 0.0558(3) 0.078(3) Uani 1 1 d .
C7 C 1.0415(6) -0.1295(5) 0.05896(18) 0.0308(12) Uani 1 1 d .
H7A H 0.9610 -0.1735 0.0550 0.046 Uiso 1 1 calc R
H7B H 1.1109 -0.1897 0.0555 0.046 Uiso 1 1 calc R
H7C H 1.0493 -0.0635 0.0353 0.046 Uiso 1 1 calc R
C8 C 0.8138(6) -0.3709(6) 0.1177(2) 0.0401(14) Uani 1 1 d .
H8A H 0.7388 -0.4202 0.1257 0.060 Uiso 1 1 calc R
H8B H 0.8621 -0.4153 0.0937 0.060 Uiso 1 1 calc R
H8C H 0.7881 -0.2882 0.1059 0.060 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Sn1 C1 99.12(19) 5_665 .
O2 Sn1 C2 107.63(18) 5_665 .
C1 Sn1 C2 150.2(2) . .
O2 Sn1 O1 90.90(13) 5_665 .
C1 Sn1 O1 95.6(2) . .
C2 Sn1 O1 96.86(18) . .
O2 Sn1 O7 79.95(14) 5_665 5_565
C1 Sn1 O7 92.9(2) . 5_565
C2 Sn1 O7 79.40(18) . 5_565
O1 Sn1 O7 168.42(15) . 5_565
O3 Sn2 O3 91.21(19) . 5_665
O3 Sn2 C7 105.11(19) . .
O3 Sn2 C7 96.43(19) 5_665 .
O3 Sn2 C7 96.43(19) . 5_665
O3 Sn2 C7 105.11(19) 5_665 5_665
C7 Sn2 C7 149.1(3) . 5_665
O3 Sn2 O6 79.54(13) . 5_665
O3 Sn2 O6 167.97(13) 5_665 5_665
C7 Sn2 O6 78.80(18) . 5_665
C7 Sn2 O6 83.74(18) 5_665 5_665
O3 Sn2 O6 167.97(13) . .
O3 Sn2 O6 79.54(13) 5_665 .
C7 Sn2 O6 83.74(18) . .
C7 Sn2 O6 78.80(19) 5_665 .
O6 Sn2 O6 110.61(17) 5_665 .
O1 P O3 111.6(2) . .
O1 P O2 111.1(2) . .
O3 P O2 110.5(2) . .
O1 P C3 107.4(2) . .
O3 P C3 109.9(2) . .
O2 P C3 106.2(2) . .
O8 S O6 115.3(2) . .
O8 S O7 111.9(2) . .
O6 S O7 109.2(2) . .
O8 S C8 108.3(3) . .
O6 S C8 105.0(3) . .
O7 S C8 106.5(3) . .
P O1 Sn1 133.5(2) . .
P O2 Sn1 133.8(2) . 5_665
P O3 Sn2 135.4(2) . .
C5 O5 C6 117.2(6) . .
S O6 Sn2 136.0(2) . .
S O7 Sn1 140.1(2) . 5_655
Sn1 C1 H1A 109.5 . .
Sn1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Sn1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Sn1 C2 H2A 109.5 . .
Sn1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Sn1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 C3 P 114.3(4) . .
C4 C3 H3A 108.7 . .
P C3 H3A 108.7 . .
C4 C3 H3B 108.7 . .
P C3 H3B 108.7 . .
H3A C3 H3B 107.6 . .
C5 C4 C3 112.1(5) . .
C5 C4 H4A 109.2 . .
C3 C4 H4A 109.2 . .
C5 C4 H4B 109.2 . .
C3 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
O4 C5 O5 123.3(6) . .
O4 C5 C4 125.3(6) . .
O5 C5 C4 111.3(5) . .
Sn2 C7 H7A 109.5 . .
Sn2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Sn2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
S C8 H8A 109.5 . .
S C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
S C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O2 2.058(3) 5_665
Sn1 C1 2.079(5) .
Sn1 C2 2.087(5) .
Sn1 O1 2.097(3) .
Sn1 O7 2.362(4) 5_565
Sn2 O3 2.081(3) .
Sn2 O3 2.081(3) 5_665
Sn2 C7 2.084(5) .
Sn2 C7 2.084(5) 5_665
Sn2 O6 2.556(4) 5_665
Sn2 O6 2.556(4) .
P O1 1.524(3) .
P O3 1.530(4) .
P O2 1.535(4) .
P C3 1.791(5) .
S O8 1.449(4) .
S O6 1.461(4) .
S O7 1.470(4) .
S C8 1.779(6) .
O2 Sn1 2.058(3) 5_665
O4 C5 1.203(8) .
O5 C5 1.320(8) .
O5 C6 1.457(8) .
O7 Sn1 2.362(4) 5_655
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.518(7) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.503(8) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
