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#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305291.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_4305291
loop_
_publ_author_name
'Ravi Shankar'
'Atul Pratap Singh'
'Archana Jain'
'Mary F. Mahon'
'Kieran C. Molloy'
_publ_section_title
;
Synthesis, Characterization, and Structural Studies of Mixed-Ligand
Diorganotin Esters, [R2Sn(OP(O)(OH)Ph)(OS(O)2R1)]n [R =n-Bu, R1= Me (1), n-Pr
(2); R = Et, R1= Me (3)] with 1D and 3D Coordination Polymeric Motifs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5930
_journal_page_last               5935
_journal_paper_doi               10.1021/ic8002433
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C11 H19 O6 P S Sn'
_chemical_formula_sum            'C11 H19 O6 P S Sn'
_chemical_formula_weight         429.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.9260(10)
_cell_angle_beta                 67.4340(10)
_cell_angle_gamma                69.5950(10)
_cell_formula_units_Z            2
_cell_length_a                   8.65210(10)
_cell_length_b                   9.96560(10)
_cell_length_c                   10.7760(2)
_cell_measurement_reflns_used    10734
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     790.34(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '229 2.0 degree images with 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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16259
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  0.7592
_exptl_absorpt_correction_T_min  0.6992
_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    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.733
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0195P)²+0.3652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                4411
_reflns_number_total             4615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002433-file007_3.cif
_cod_data_source_block           k07kcm51
_cod_original_cell_volume        790.340(19)
_cod_database_code               4305291
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn Sn 0.925996(13) 0.766764(10) 0.546221(10) 0.01580(5) Uani 1 1 d . . .
S S 1.02781(6) 1.02743(5) 0.22942(4) 0.02366(10) Uani 1 1 d . . .
P P 0.99991(6) 0.58740(4) 0.28493(4) 0.01728(9) Uani 1 1 d . . .
O1 O 0.89836(18) 0.96649(14) 0.34760(13) 0.0259(3) Uani 1 1 d . . .
O2 O 1.1078(2) 1.10956(18) 0.26689(16) 0.0356(3) Uani 1 1 d . . .
O3 O 1.1560(2) 0.91728(16) 0.15110(15) 0.0330(3) Uani 1 1 d . . .
O4 O 0.92885(18) 0.64855(13) 0.41425(13) 0.0222(3) Uani 1 1 d . . .
O5 O 1.15663(18) 0.64603(16) 0.17965(14) 0.0263(3) Uani 1 1 d . . .
H5 H 1.147(4) 0.726(3) 0.174(3) 0.049(9) Uiso 1 1 d . . .
O6 O 1.06496(18) 0.42362(13) 0.30353(13) 0.0240(3) Uani 1 1 d . . .
C1 C 0.6540(2) 0.8540(2) 0.6169(2) 0.0306(4) Uani 1 1 d . . .
H1A H 0.6200 0.8596 0.7144 0.037 Uiso 0.663(7) 1 calc PR A 1
H1B H 0.6251 0.9549 0.5661 0.037 Uiso 0.663(7) 1 calc PR A 1
H1C H 0.6306 0.9484 0.6426 0.037 Uiso 0.337(7) 1 calc PR A 2
H1D H 0.6091 0.8748 0.5395 0.037 Uiso 0.337(7) 1 calc PR A 2
C2 C 0.5472(4) 0.7743(5) 0.6046(4) 0.0435(11) Uani 0.663(7) 1 d P A 1
H2A H 0.4239 0.8243 0.6405 0.065 Uiso 0.663(7) 1 calc PR A 1
H2B H 0.5708 0.6749 0.6570 0.065 Uiso 0.663(7) 1 calc PR A 1
H2C H 0.5757 0.7707 0.5082 0.065 Uiso 0.663(7) 1 calc PR A 1
C2A C 0.5592(10) 0.7704(11) 0.7264(10) 0.064(3) Uani 0.337(7) 1 d P A 2
H2D H 0.4359 0.8237 0.7504 0.096 Uiso 0.337(7) 1 calc PR A 2
H2E H 0.6000 0.7497 0.8050 0.096 Uiso 0.337(7) 1 calc PR A 2
H2F H 0.5745 0.6786 0.7013 0.096 Uiso 0.337(7) 1 calc PR A 2
C3 C 1.1918(3) 0.7584(2) 0.4865(3) 0.0377(5) Uani 1 1 d . . .
H3A H 1.2118 0.8460 0.4165 0.045 Uiso 0.663(7) 1 calc PR A 1
H3B H 1.2167 0.7642 0.5668 0.045 Uiso 0.663(7) 1 calc PR A 1
H3C H 1.2272 0.7980 0.3871 0.045 Uiso 0.337(7) 1 calc PR A 2
H3D H 1.1991 0.8279 0.5321 0.045 Uiso 0.337(7) 1 calc PR A 2
C4 C 1.3180(5) 0.6288(4) 0.4310(5) 0.0319(9) Uani 0.663(7) 1 d P A 1
H4A H 1.4363 0.6366 0.4069 0.048 Uiso 0.663(7) 1 calc PR A 1
H4B H 1.2982 0.6231 0.3492 0.048 Uiso 0.663(7) 1 calc PR A 1
H4C H 1.3031 0.5409 0.5001 0.048 Uiso 0.663(7) 1 calc PR A 1
C4A C 1.3146(11) 0.6339(13) 0.5070(16) 0.078(5) Uani 0.337(7) 1 d P A 2
H4D H 1.4281 0.6544 0.4729 0.117 Uiso 0.337(7) 1 calc PR A 2
H4E H 1.3176 0.5639 0.4580 0.117 Uiso 0.337(7) 1 calc PR A 2
H4F H 1.2875 0.5929 0.6050 0.117 Uiso 0.337(7) 1 calc PR A 2
C5 C 0.9145(3) 1.1512(2) 0.1194(2) 0.0367(5) Uani 1 1 d . . .
H5A H 0.8237 1.2268 0.1679 0.055 Uiso 1 1 calc R . .
H5B H 0.8612 1.0996 0.0893 0.055 Uiso 1 1 calc R . .
H5C H 0.9952 1.1964 0.0397 0.055 Uiso 1 1 calc R . .
C6 C 0.8321(2) 0.64692(19) 0.20730(17) 0.0197(3) Uani 1 1 d . . .
C7 C 0.7170(3) 0.7858(2) 0.2123(2) 0.0256(4) Uani 1 1 d . . .
H7 H 0.7243 0.8480 0.2606 0.031 Uiso 1 1 calc R . .
C8 C 0.5918(3) 0.8330(2) 0.1468(2) 0.0358(5) Uani 1 1 d . . .
H8 H 0.5137 0.9275 0.1502 0.043 Uiso 1 1 calc R . .
C9 C 0.5809(3) 0.7424(3) 0.0765(3) 0.0420(5) Uani 1 1 d . . .
H9 H 0.4949 0.7748 0.0322 0.050 Uiso 1 1 calc R . .
C10 C 0.6950(3) 0.6045(3) 0.0704(3) 0.0424(5) Uani 1 1 d . . .
H10 H 0.6879 0.5431 0.0212 0.051 Uiso 1 1 calc R . .
C11 C 0.8197(3) 0.5565(2) 0.1365(2) 0.0309(4) Uani 1 1 d . . .
H11 H 0.8968 0.4616 0.1333 0.037 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
_geom_angle_publ_flag
O4 Sn O6 88.81(5) . 2_766 ?
O4 Sn C1 96.87(7) . . ?
O6 Sn C1 96.08(7) 2_766 . ?
O4 Sn C3 101.49(7) . . ?
O6 Sn C3 96.46(8) 2_766 . ?
C1 Sn C3 157.92(9) . . ?
O4 Sn O1 80.79(5) . . ?
O6 Sn O1 169.13(5) 2_766 . ?
C1 Sn O1 82.12(7) . . ?
C3 Sn O1 88.78(8) . . ?
O4 Sn O2 171.67(5) . 2_776 ?
O6 Sn O2 84.94(5) 2_766 2_776 ?
C1 Sn O2 78.36(7) . 2_776 ?
C3 Sn O2 84.73(8) . 2_776 ?
O1 Sn O2 105.08(5) . 2_776 ?
O2 S O3 112.35(9) . . ?
O2 S O1 112.66(9) . . ?
O3 S O1 112.20(8) . . ?
O2 S C5 106.73(11) . . ?
O3 S C5 105.88(10) . . ?
O1 S C5 106.44(10) . . ?
O4 P O6 115.27(7) . . ?
O4 P O5 111.56(8) . . ?
O6 P O5 105.67(8) . . ?
O4 P C6 108.01(8) . . ?
O6 P C6 108.74(8) . . ?
O5 P C6 107.30(8) . . ?
S O1 Sn 132.38(8) . . ?
S O2 Sn 143.30(9) . 2_776 ?
P O4 Sn 154.87(9) . . ?
P O5 H5 115(2) . . ?
P O6 Sn 142.55(8) . 2_766 ?
C2A C1 C2 56.0(5) . . ?
C2A C1 Sn 117.5(4) . . ?
C2 C1 Sn 116.60(18) . . ?
C2A C1 H1A 54.2 . . ?
C2 C1 H1A 108.1 . . ?
Sn C1 H1A 108.1 . . ?
C2A C1 H1B 134.0 . . ?
C2 C1 H1B 108.1 . . ?
Sn C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C2A C1 H1C 107.9 . . ?
C2 C1 H1C 135.1 . . ?
Sn C1 H1C 107.9 . . ?
H1A C1 H1C 60.3 . . ?
H1B C1 H1C 49.4 . . ?
C2A C1 H1D 107.9 . . ?
C2 C1 H1D 54.5 . . ?
Sn C1 H1D 107.9 . . ?
H1A C1 H1D 143.9 . . ?
H1B C1 H1D 60.0 . . ?
H1C C1 H1D 107.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2A H2D 109.5 . . ?
C1 C2A H2E 109.5 . . ?
H2D C2A H2E 109.5 . . ?
C1 C2A H2F 109.5 . . ?
H2D C2A H2F 109.5 . . ?
H2E C2A H2F 109.5 . . ?
C4A C3 Sn 122.7(4) . . ?
C4 C3 Sn 116.56(18) . . ?
C4A C3 H3A 125.7 . . ?
C4 C3 H3A 108.2 . . ?
Sn C3 H3A 108.2 . . ?
C4A C3 H3B 75.4 . . ?
C4 C3 H3B 108.2 . . ?
Sn C3 H3B 108.2 . . ?
H3A C3 H3B 107.3 . . ?
C4A C3 H3C 106.6 . . ?
C4 C3 H3C 78.4 . . ?
Sn C3 H3C 106.6 . . ?
H3B C3 H3C 136.1 . . ?
C4A C3 H3D 106.6 . . ?
C4 C3 H3D 133.1 . . ?
Sn C3 H3D 106.6 . . ?
H3A C3 H3D 72.6 . . ?
H3C C3 H3D 106.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C4A H4D 109.5 . . ?
C3 C4A H4E 109.5 . . ?
H4D C4A H4E 109.5 . . ?
C3 C4A H4F 109.5 . . ?
H4D C4A H4F 109.5 . . ?
H4E C4A H4F 109.5 . . ?
S C5 H5A 109.5 . . ?
S C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
S C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 119.37(17) . . ?
C11 C6 P 119.89(14) . . ?
C7 C6 P 120.69(14) . . ?
C8 C7 C6 120.15(18) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.4(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 119.9(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C6 120.3(2) . . ?
C10 C11 H11 119.9 . . ?
C6 C11 H11 119.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn O4 2.0850(12) . ?
Sn O6 2.1017(12) 2_766 ?
Sn C1 2.1122(18) . ?
Sn C3 2.1143(19) . ?
Sn O1 2.4818(13) . ?
Sn O2 2.5328(14) 2_776 ?
S O2 1.4543(15) . ?
S O3 1.4574(15) . ?
S O1 1.4733(14) . ?
S C5 1.754(2) . ?
P O4 1.5070(13) . ?
P O6 1.5083(13) . ?
P O5 1.5651(14) . ?
P C6 1.7887(18) . ?
O2 Sn 2.5328(14) 2_776 ?
O5 H5 0.76(3) . ?
O6 Sn 2.1017(12) 2_766 ?
C1 C2A 1.384(8) . ?
C1 C2 1.473(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2A H2D 0.9800 . ?
C2A H2E 0.9800 . ?
C2A H2F 0.9800 . ?
C3 C4A 1.348(9) . ?
C3 C4 1.479(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4A H4D 0.9800 . ?
C4A H4E 0.9800 . ?
C4A H4F 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.393(3) . ?
C6 C7 1.397(2) . ?
C7 C8 1.389(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
