#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:50:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114876.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_4114876
loop_
_publ_author_name
'Timothy J. Boyle'
'Judith M. Segall'
'Todd M. Alam'
'Mark A. Rodriguez'
'Jessica M. Santana'
_publ_section_title
;
 Chemistry of a Novel Family of Tridentate Alkoxy Tin(II) Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6904
_journal_page_last               6913
_journal_paper_doi               10.1021/ja0202309
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C24 H44 O14 Sn6'
_chemical_formula_weight         1268.73
_chemical_name_common            '[Sn3(THME)2]2 * (Diox)slovent'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 113.638(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.379(4)
_cell_length_b                   10.4956(15)
_cell_length_c                   12.4140(18)
_cell_measurement_temperature    168(2)
_cell_volume                     3626.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11073
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    4.128
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0271P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                2402
_reflns_number_total             2609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0202309_05.cif
_cod_data_source_block           tjb089q_structure_1e_Dioxane
_cod_database_code               4114876
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.574649(8) 0.28625(2) 0.178932(19) 0.03055(8) Uani 1 1 d .
Sn2 Sn 0.686268(8) 0.42508(2) 0.330522(18) 0.02936(8) Uani 1 1 d .
Sn3 Sn 0.656151(8) 0.31206(2) 0.048286(19) 0.03050(8) Uani 1 1 d .
O1 O 0.64171(8) 0.2622(2) 0.33582(18) 0.0294(5) Uani 1 1 d .
O2 O 0.61727(7) 0.1711(2) 0.10907(17) 0.0305(5) Uani 1 1 d .
O3 O 0.70681(7) 0.28153(19) 0.23092(19) 0.0297(5) Uani 1 1 d .
O4 O 0.60875(7) 0.4673(2) 0.25828(17) 0.0284(5) Uani 1 1 d .
O5 O 0.58497(8) 0.3763(2) 0.03068(17) 0.0299(5) Uani 1 1 d .
O6 O 0.67397(7) 0.4868(2) 0.15348(17) 0.0276(5) Uani 1 1 d .
C1 C 0.66297(12) 0.1401(3) 0.3719(3) 0.0351(8) Uani 1 1 d .
H1A H 0.6391 0.0835 0.3830 0.042 Uiso 1 1 calc R
H1B H 0.6904 0.1491 0.4490 0.042 Uiso 1 1 calc R
C2 C 0.63970(13) 0.0575(3) 0.1671(3) 0.0355(8) Uani 1 1 d .
H2A H 0.6522 0.0111 0.1159 0.043 Uiso 1 1 calc R
H2B H 0.6150 0.0028 0.1771 0.043 Uiso 1 1 calc R
C3 C 0.72100(12) 0.1565(3) 0.2756(3) 0.0360(8) Uani 1 1 d .
H3A H 0.7478 0.1630 0.3540 0.043 Uiso 1 1 calc R
H3B H 0.7332 0.1112 0.2231 0.043 Uiso 1 1 calc R
C4 C 0.68074(12) 0.0766(3) 0.2870(3) 0.0314(8) Uani 1 1 d .
C5 C 0.70131(14) -0.0542(3) 0.3355(3) 0.0418(9) Uani 1 1 d .
H5A H 0.7255 -0.0449 0.4161 0.063 Uiso 1 1 calc R
H5B H 0.7162 -0.0918 0.2861 0.063 Uiso 1 1 calc R
H5C H 0.6754 -0.1098 0.3355 0.063 Uiso 1 1 calc R
C6 C 0.58906(12) 0.5843(3) 0.1991(3) 0.0312(8) Uani 1 1 d .
H6A H 0.6040 0.6561 0.2532 0.037 Uiso 1 1 calc R
H6B H 0.5542 0.5858 0.1806 0.037 Uiso 1 1 calc R
C7 C 0.57021(11) 0.5037(3) -0.0057(3) 0.0314(8) Uani 1 1 d .
H7A H 0.5353 0.5108 -0.0257 0.038 Uiso 1 1 calc R
H7B H 0.5754 0.5214 -0.0781 0.038 Uiso 1 1 calc R
C8 C 0.64986(12) 0.6061(3) 0.1111(3) 0.0328(8) Uani 1 1 d .
H8A H 0.6537 0.6293 0.0380 0.039 Uiso 1 1 calc R
H8B H 0.6658 0.6729 0.1702 0.039 Uiso 1 1 calc R
C9 C 0.59633(12) 0.6051(3) 0.0858(3) 0.0297(7) Uani 1 1 d .
C10 C 0.57573(13) 0.7345(3) 0.0346(3) 0.0398(9) Uani 1 1 d .
H10A H 0.5412 0.7361 0.0167 0.060 Uiso 1 1 calc R
H10B H 0.5807 0.7492 -0.0376 0.060 Uiso 1 1 calc R
H10C H 0.5920 0.8014 0.0919 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'
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
O2 Sn1 O1 78.58(8)
O2 Sn1 O4 114.03(8)
O1 Sn1 O4 66.39(8)
O2 Sn1 O5 66.43(8)
O1 Sn1 O5 113.49(8)
O4 Sn1 O5 78.70(7)
O6 Sn2 O3 66.88(8)
O6 Sn2 O1 113.80(8)
O3 Sn2 O1 78.48(8)
O6 Sn2 O4 78.83(7)
O3 Sn2 O4 114.08(8)
O1 Sn2 O4 66.29(8)
O6 Sn3 O5 78.46(8)
O6 Sn3 O3 66.60(8)
O5 Sn3 O3 113.79(8)
O6 Sn3 O2 113.31(8)
O5 Sn3 O2 66.30(8)
O3 Sn3 O2 78.38(8)
C1 O1 Sn1 121.66(19)
C1 O1 Sn2 120.14(19)
Sn1 O1 Sn2 104.31(9)
C2 O2 Sn1 120.20(19)
C2 O2 Sn3 121.57(19)
Sn1 O2 Sn3 104.38(9)
C3 O3 Sn2 121.62(19)
C3 O3 Sn3 121.00(19)
Sn2 O3 Sn3 104.01(9)
C6 O4 Sn1 119.09(17)
C6 O4 Sn2 122.63(18)
Sn1 O4 Sn2 104.10(9)
C7 O5 Sn3 119.53(18)
C7 O5 Sn1 122.39(18)
Sn3 O5 Sn1 104.50(9)
C8 O6 Sn2 119.00(17)
C8 O6 Sn3 122.85(18)
Sn2 O6 Sn3 104.74(9)
O1 C1 C4 114.8(3)
O2 C2 C4 115.0(3)
O3 C3 C4 114.3(3)
C1 C4 C2 110.9(3)
C1 C4 C5 108.9(3)
C2 C4 C5 108.1(3)
C1 C4 C3 110.0(3)
C2 C4 C3 110.6(3)
C5 C4 C3 108.2(3)
O4 C6 C9 114.2(3)
O5 C7 C9 114.5(3)
O6 C8 C9 114.4(3)
C10 C9 C6 109.0(3)
C10 C9 C7 107.9(3)
C6 C9 C7 111.2(3)
C10 C9 C8 107.8(3)
C6 C9 C8 110.3(3)
C7 C9 C8 110.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn1 O2 2.189(2)
Sn1 O1 2.197(2)
Sn1 O4 2.199(2)
Sn1 O5 2.200(2)
Sn2 O6 2.175(2)
Sn2 O3 2.193(2)
Sn2 O1 2.198(2)
Sn2 O4 2.203(2)
Sn3 O6 2.190(2)
Sn3 O5 2.191(2)
Sn3 O3 2.194(2)
Sn3 O2 2.206(2)
O1 C1 1.423(4)
O2 C2 1.419(4)
O3 C3 1.423(4)
O4 C6 1.433(4)
O5 C7 1.425(4)
O6 C8 1.439(4)
C1 C4 1.517(5)
C2 C4 1.524(5)
C3 C4 1.535(5)
C4 C5 1.529(5)
C6 C9 1.525(4)
C7 C9 1.526(4)
C8 C9 1.528(4)
C9 C10 1.523(5)
