#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:50:55 +0100 (mar 22 de mar de 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114875.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_4114875
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            'C35 H59 N O18 Sn9'
_chemical_formula_weight         1850.04
_chemical_name_common            '[Sn(THME)2]3 * (Py)solvent'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   22.278(4)
_cell_length_b                   10.0634(16)
_cell_length_c                   23.648(4)
_cell_measurement_temperature    168(2)
_cell_volume                     5301.7(16)
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32253
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    4.228
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_description       roundish
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          .2
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0234
_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)+(0.0328P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                3563
_reflns_number_total             4071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0202309_04.cif
_cod_data_source_block           tjb088p_structure_1d_Pyridine
_cod_original_cell_volume        5301.7(15)
_cod_database_code               4114875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.206860(18) 0.7500 0.850350(16) 0.03068(11) Uani 1 2 d S
Sn2 Sn 0.275719(14) 0.92233(3) 0.740535(13) 0.03769(10) Uani 1 1 d .
Sn3 Sn 0.152412(16) 0.07699(3) 0.543987(13) 0.04450(11) Uani 1 1 d .
Sn4 Sn 0.16497(2) 0.2500 0.670541(17) 0.04171(13) Uani 1 2 d S
Sn5 Sn 0.391941(14) 0.92173(3) 0.456664(12) 0.03361(10) Uani 1 1 d .
Sn6 Sn 0.294418(18) 0.7500 0.545249(16) 0.03113(11) Uani 1 2 d S
O1 O 0.18754(12) 0.8899(3) 0.78193(11) 0.0335(7) Uani 1 1 d .
O2 O 0.24272(18) 0.7500 0.69446(15) 0.0372(10) Uani 1 2 d S
O3 O 0.28161(12) 0.8865(3) 0.83181(11) 0.0310(7) Uani 1 1 d .
O4 O 0.33732(17) 0.7500 0.74362(15) 0.0351(10) Uani 1 2 d S
O5 O 0.10547(15) 0.1118(3) 0.62477(12) 0.0464(8) Uani 1 1 d .
O6 O 0.0957(2) 0.2500 0.52279(17) 0.0464(11) Uani 1 2 d S
O7 O 0.21295(14) 0.1118(3) 0.61489(12) 0.0381(7) Uani 1 1 d .
O8 O 0.20241(19) 0.2500 0.51290(16) 0.0407(11) Uani 1 2 d S
O9 O 0.29675(12) 0.8887(2) 0.47321(11) 0.0287(6) Uani 1 1 d .
O10 O 0.37452(17) 0.7500 0.40187(15) 0.0313(9) Uani 1 2 d S
O11 O 0.37148(12) 0.8883(3) 0.54669(11) 0.0317(7) Uani 1 1 d .
O12 O 0.44893(16) 0.7500 0.47608(16) 0.0328(9) Uani 1 2 d S
C1 C 0.13444(19) 0.8748(5) 0.74864(18) 0.0385(11) Uani 1 1 d .
H1A H 0.1305 0.9532 0.7236 0.046 Uiso 1 1 calc R
H1B H 0.0993 0.8742 0.7743 0.046 Uiso 1 1 calc R
C2 C 0.1836(3) 0.7500 0.6700(3) 0.0406(16) Uani 1 2 d S
H2A H 0.1796 0.6707 0.6456 0.049 Uiso 0.50 1 calc PR
H2B H 0.1796 0.8293 0.6456 0.049 Uiso 0.50 1 calc PR
C3 C 0.1325(3) 0.7500 0.7123(2) 0.0352(15) Uani 1 2 d S
C4 C 0.0734(3) 0.7500 0.6793(3) 0.0532(19) Uani 1 2 d S
H4A H 0.0713 0.6702 0.6556 0.080 Uiso 0.50 1 calc PR
H4B H 0.0715 0.8293 0.6552 0.080 Uiso 0.50 1 calc PR
H4C H 0.0396 0.7505 0.7058 0.080 Uiso 1 2 calc SR
C5 C 0.33791(18) 0.8743(4) 0.85926(18) 0.0353(10) Uani 1 1 d .
H5A H 0.3312 0.8741 0.9006 0.042 Uiso 1 1 calc R
H5B H 0.3625 0.9533 0.8501 0.042 Uiso 1 1 calc R
C6 C 0.3881(3) 0.7500 0.7805(2) 0.0400(16) Uani 1 2 d S
H6A H 0.4128 0.8293 0.7721 0.048 Uiso 0.50 1 calc PR
H6B H 0.4128 0.6707 0.7721 0.048 Uiso 0.50 1 calc PR
C7 C 0.3732(3) 0.7500 0.8434(2) 0.0318(14) Uani 1 2 d S
C8 C 0.4317(3) 0.7500 0.8772(3) 0.0416(16) Uani 1 2 d S
H8A H 0.4226 0.7500 0.9177 0.062 Uiso 1 2 calc SR
H8B H 0.4551 0.8295 0.8678 0.062 Uiso 0.50 1 calc PR
H8C H 0.4551 0.6705 0.8678 0.062 Uiso 0.50 1 calc PR
C9 C 0.0417(2) 0.1249(5) 0.6261(2) 0.0585(14) Uani 1 1 d .
H9A H 0.0284 0.1249 0.6661 0.070 Uiso 1 1 calc R
H9B H 0.0237 0.0460 0.6076 0.070 Uiso 1 1 calc R
C10 C 0.0335(3) 0.2500 0.5337(3) 0.057(2) Uani 1 2 d S
H10A H 0.0155 0.1706 0.5158 0.068 Uiso 0.50 1 calc PR
H10B H 0.0155 0.3294 0.5158 0.068 Uiso 0.50 1 calc PR
C11 C 0.0172(3) 0.2500 0.5972(3) 0.057(2) Uani 1 2 d S
C12 C -0.0516(3) 0.2500 0.6034(3) 0.077(3) Uani 1 2 d S
H12A H -0.0683 0.3281 0.5843 0.116 Uiso 0.50 1 calc PR
H12B H -0.0623 0.2527 0.6436 0.116 Uiso 1 2 calc SR
H12C H -0.0681 0.1692 0.5863 0.116 Uiso 0.50 1 calc PR
C13 C 0.2764(2) 0.1259(4) 0.60538(19) 0.0421(12) Uani 1 1 d .
H13A H 0.2908 0.0472 0.5842 0.051 Uiso 1 1 calc R
H13B H 0.2970 0.1263 0.6425 0.051 Uiso 1 1 calc R
C14 C 0.2669(3) 0.2500 0.5140(2) 0.0390(16) Uani 1 2 d S
H14A H 0.2814 0.3293 0.4934 0.047 Uiso 0.50 1 calc PR
H14B H 0.2814 0.1707 0.4934 0.047 Uiso 0.50 1 calc PR
C15 C 0.2946(3) 0.2500 0.5731(2) 0.0345(15) Uani 1 2 d S
C16 C 0.3625(3) 0.2500 0.5667(3) 0.0454(17) Uani 1 2 d S
H16A H 0.3812 0.2500 0.6042 0.068 Uiso 1 2 calc SR
H16B H 0.3750 0.3295 0.5459 0.068 Uiso 0.50 1 calc PR
H16C H 0.3750 0.1705 0.5459 0.068 Uiso 0.50 1 calc PR
C17 C 0.25498(19) 0.8749(4) 0.42759(17) 0.0350(10) Uani 1 1 d .
H17A H 0.2583 0.9538 0.4028 0.042 Uiso 1 1 calc R
H17B H 0.2138 0.8736 0.4433 0.042 Uiso 1 1 calc R
C18 C 0.3247(3) 0.7500 0.3629(2) 0.0358(15) Uani 1 2 d S
H18A H 0.3276 0.6706 0.3384 0.043 Uiso 0.50 1 calc PR
H18B H 0.3276 0.8294 0.3384 0.043 Uiso 0.50 1 calc PR
C19 C 0.2642(3) 0.7500 0.3917(2) 0.0303(14) Uani 1 2 d S
C20 C 0.2154(3) 0.7500 0.3455(3) 0.0392(16) Uani 1 2 d S
H20A H 0.2200 0.6710 0.3217 0.059 Uiso 0.50 1 calc PR
H20B H 0.2194 0.8300 0.3222 0.059 Uiso 0.50 1 calc PR
H20C H 0.1756 0.7490 0.3633 0.059 Uiso 1 2 calc SR
C21 C 0.41743(19) 0.8751(4) 0.58808(18) 0.0391(11) Uani 1 1 d .
H21A H 0.3986 0.8733 0.6260 0.047 Uiso 1 1 calc R
H21B H 0.4437 0.9543 0.5863 0.047 Uiso 1 1 calc R
C22 C 0.4882(3) 0.7500 0.5246(3) 0.0404(16) Uani 1 2 d S
H22A H 0.5144 0.8294 0.5226 0.049 Uiso 0.50 1 calc PR
H22B H 0.5144 0.6706 0.5226 0.049 Uiso 0.50 1 calc PR
C23 C 0.4564(3) 0.7500 0.5811(2) 0.0353(15) Uani 1 2 d S
C24 C 0.5041(3) 0.7500 0.6283(3) 0.0480(18) Uani 1 2 d S
H24A H 0.4841 0.7500 0.6653 0.072 Uiso 1 2 calc SR
H24B H 0.5292 0.8295 0.6249 0.072 Uiso 0.50 1 calc PR
H24C H 0.5292 0.6705 0.6249 0.072 Uiso 0.50 1 calc PR
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'
N N 0.0061 0.0033 '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
O1 Sn1 O1 80.12(14) 7_575 .
O1 Sn1 O3 113.75(10) 7_575 .
O1 Sn1 O3 66.43(10) . .
O1 Sn1 O3 66.43(10) 7_575 7_575
O1 Sn1 O3 113.75(10) . 7_575
O3 Sn1 O3 77.16(14) . 7_575
O2 Sn2 O3 112.47(11) . .
O2 Sn2 O4 66.51(12) . .
O3 Sn2 O4 78.55(12) . .
O2 Sn2 O1 78.73(12) . .
O3 Sn2 O1 66.07(10) . .
O4 Sn2 O1 114.79(11) . .
O7 Sn3 O8 79.39(13) . .
O7 Sn3 O5 66.53(12) . .
O8 Sn3 O5 113.88(12) . .
O7 Sn3 O6 113.68(12) . .
O8 Sn3 O6 65.73(14) . .
O5 Sn3 O6 78.47(14) . .
O7 Sn4 O7 78.70(14) . 7_565
O7 Sn4 O5 66.33(11) . .
O7 Sn4 O5 113.47(11) 7_565 .
O7 Sn4 O5 113.47(11) . 7_565
O7 Sn4 O5 66.33(11) 7_565 7_565
O5 Sn4 O5 78.20(17) . 7_565
O9 Sn5 O12 113.90(11) . .
O9 Sn5 O10 79.29(12) . .
O12 Sn5 O10 66.76(12) . .
O9 Sn5 O11 66.57(10) . .
O12 Sn5 O11 78.30(12) . .
O10 Sn5 O11 114.44(11) . .
O9 Sn6 O9 78.65(13) 7_575 .
O9 Sn6 O11 113.12(10) 7_575 .
O9 Sn6 O11 66.08(10) . .
O9 Sn6 O11 66.08(10) 7_575 7_575
O9 Sn6 O11 113.12(10) . 7_575
O11 Sn6 O11 78.06(14) . 7_575
C1 O1 Sn1 120.1(2) . .
C1 O1 Sn2 120.4(2) . .
Sn1 O1 Sn2 104.29(11) . .
C2 O2 Sn2 120.70(15) . .
C2 O2 Sn2 120.70(15) . 7_575
Sn2 O2 Sn2 105.68(16) . 7_575
C5 O3 Sn2 121.2(2) . .
C5 O3 Sn1 121.6(2) . .
Sn2 O3 Sn1 104.67(11) . .
C6 O4 Sn2 120.73(15) . 7_575
C6 O4 Sn2 120.73(15) . .
Sn2 O4 Sn2 103.21(15) 7_575 .
C9 O5 Sn4 122.0(3) . .
C9 O5 Sn3 120.4(3) . .
Sn4 O5 Sn3 103.91(13) . .
C10 O6 Sn3 121.39(17) . 7_565
C10 O6 Sn3 121.39(17) . .
Sn3 O6 Sn3 104.02(18) 7_565 .
C13 O7 Sn3 120.2(2) . .
C13 O7 Sn4 120.7(3) . .
Sn3 O7 Sn4 105.19(13) . .
C14 O8 Sn3 120.09(16) . .
C14 O8 Sn3 120.09(16) . 7_565
Sn3 O8 Sn3 105.06(17) . 7_565
C17 O9 Sn5 120.8(2) . .
C17 O9 Sn6 120.4(2) . .
Sn5 O9 Sn6 104.96(11) . .
C18 O10 Sn5 120.87(15) . .
C18 O10 Sn5 120.87(15) . 7_575
Sn5 O10 Sn5 103.90(15) . 7_575
C21 O11 Sn5 122.0(2) . .
C21 O11 Sn6 120.7(2) . .
Sn5 O11 Sn6 104.00(11) . .
C22 O12 Sn5 121.16(15) . 7_575
C22 O12 Sn5 121.16(15) . .
Sn5 O12 Sn5 104.01(15) 7_575 .
O1 C1 C3 115.0(4) . .
O2 C2 C3 115.0(5) . .
C2 C3 C1 110.5(3) . 7_575
C2 C3 C1 110.5(3) . .
C1 C3 C1 111.2(5) 7_575 .
C2 C3 C4 108.0(5) . .
C1 C3 C4 108.2(3) 7_575 .
C1 C3 C4 108.2(3) . .
O3 C5 C7 114.6(4) . .
O4 C6 C7 115.2(5) . .
C6 C7 C5 110.6(3) . 7_575
C6 C7 C5 110.6(3) . .
C5 C7 C5 110.2(5) 7_575 .
C6 C7 C8 109.0(5) . .
C5 C7 C8 108.1(3) 7_575 .
C5 C7 C8 108.1(3) . .
O5 C9 C11 114.8(5) . .
O6 C10 C11 114.2(6) . .
C9 C11 C9 110.5(6) 7_565 .
C9 C11 C12 108.2(4) 7_565 .
C9 C11 C12 108.2(4) . .
C9 C11 C10 110.4(4) 7_565 .
C9 C11 C10 110.4(4) . .
C12 C11 C10 109.1(6) . .
O7 C13 C15 114.9(4) . .
O8 C14 C15 114.9(5) . .
C13 C15 C13 110.6(5) 7_565 .
C13 C15 C16 108.4(4) 7_565 .
C13 C15 C16 108.4(4) . .
C13 C15 C14 110.6(3) 7_565 .
C13 C15 C14 110.6(3) . .
C16 C15 C14 108.2(5) . .
O9 C17 C19 114.2(4) . .
O10 C18 C19 113.5(5) . .
C18 C19 C17 111.7(3) . .
C18 C19 C17 111.7(3) . 7_575
C17 C19 C17 110.5(5) . 7_575
C18 C19 C20 108.0(5) . .
C17 C19 C20 107.4(3) . .
C17 C19 C20 107.4(3) 7_575 .
O11 C21 C23 114.2(4) . .
O12 C22 C23 114.8(5) . .
C22 C23 C21 111.0(3) . 7_575
C22 C23 C21 111.0(3) . .
C21 C23 C21 109.8(5) 7_575 .
C22 C23 C24 108.5(5) . .
C21 C23 C24 108.2(3) 7_575 .
C21 C23 C24 108.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O1 2.187(3) 7_575
Sn1 O1 2.187(3) .
Sn1 O3 2.203(3) .
Sn1 O3 2.203(3) 7_575
Sn2 O2 2.176(2) .
Sn2 O3 2.192(3) .
Sn2 O4 2.213(2) .
Sn2 O1 2.219(3) .
Sn3 O7 2.180(3) .
Sn3 O8 2.194(3) .
Sn3 O5 2.206(3) .
Sn3 O6 2.209(3) .
Sn4 O7 2.193(3) .
Sn4 O7 2.193(3) 7_565
Sn4 O5 2.205(3) .
Sn4 O5 2.205(3) 7_565
Sn5 O9 2.182(3) .
Sn5 O12 2.193(2) .
Sn5 O10 2.195(2) .
Sn5 O11 2.203(3) .
Sn6 O9 2.203(3) 7_575
Sn6 O9 2.203(3) .
Sn6 O11 2.210(3) .
Sn6 O11 2.210(3) 7_575
O1 C1 1.429(5) .
O2 C2 1.438(7) .
O2 Sn2 2.176(2) 7_575
O3 C5 1.418(5) .
O4 C6 1.428(7) .
O4 Sn2 2.213(2) 7_575
O5 C9 1.428(6) .
O6 C10 1.408(8) .
O6 Sn3 2.209(3) 7_565
O7 C13 1.439(5) .
O8 C14 1.436(7) .
O8 Sn3 2.194(3) 7_565
O9 C17 1.432(5) .
O10 C18 1.443(7) .
O10 Sn5 2.195(2) 7_575
O11 C21 1.422(5) .
O12 C22 1.443(7) .
O12 Sn5 2.193(2) 7_575
C1 C3 1.523(5) .
C2 C3 1.516(8) .
C3 C1 1.523(5) 7_575
C3 C4 1.530(8) .
C5 C7 1.525(5) .
C6 C7 1.523(8) .
C7 C5 1.525(5) 7_575
C7 C8 1.529(8) .
C9 C11 1.533(6) .
C10 C11 1.546(9) .
C11 C9 1.533(6) 7_565
C11 C12 1.539(10) .
C13 C15 1.519(5) .
C14 C15 1.527(9) .
C15 C13 1.519(5) 7_565
C15 C16 1.520(8) .
C17 C19 1.530(5) .
C18 C19 1.510(8) .
C19 C17 1.530(5) 7_575
C19 C20 1.541(8) .
C21 C23 1.538(5) .
C22 C23 1.513(8) .
C23 C21 1.538(5) 7_575
C23 C24 1.540(8) .
