#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/10/4081085.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_4081085
loop_
_publ_author_name
'Gock, Michael'
'Wiedemann, Bianca'
'Dietz, Christina'
'Bai, Chenyu'
'Lutter, Michael'
'Abeyawarathan, Vinusuya'
'Jurkschat, Klaus'
_publ_section_title
;
 Simplicity Meets Beauty. Trapping Molecular Dimethyltin Oxide in the
 Novel Organotinoxo Cluster [MeN(CH2CH2O)2SnMe2.Me2SnO]3
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4262
_journal_paper_doi               10.1021/om400432k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C27 H69 N3 O9 Sn6, o.25 (H2 O)'
_chemical_formula_sum            'C27 H69.5 N3 O9.25 Sn6'
_chemical_formula_weight         1296.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.2605(3)
_cell_length_b                   14.2605(3)
_cell_length_c                   13.0444(7)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0751
_cell_measurement_theta_min      2.2664
_cell_volume                     2297.33(14)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       'ω und ψ scan'
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14906
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    3.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1253
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0198
_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)+(0.0188P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                1239
_reflns_number_total             1496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400432k_si_002.cif
_cod_data_source_block           compound3*0.25H2O
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_original_formula_sum        'C27 H69.50 N3 O9.25 Sn6'
_cod_database_code               4081085
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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 0.62692(2) 0.15269(2) 0.7500 0.02416(9) Uani 1 2 d S
O1 O 0.7788(2) 0.30177(19) 0.7500 0.0267(7) Uani 1 2 d S
C1 C 0.6252(3) 0.1402(3) 0.5888(3) 0.0445(9) Uani 1 1 d .
H1A H 0.6544 0.2124 0.5584 0.067 Uiso 1 1 calc R
H1B H 0.5506 0.0935 0.5652 0.067 Uiso 1 1 calc R
H1C H 0.6697 0.1089 0.5678 0.067 Uiso 1 1 calc R
Sn2 Sn 0.89965(2) 0.26668(2) 0.7500 0.03533(11) Uani 1 2 d S
C2 C 0.9614(3) 0.2472(3) 0.6088(3) 0.0699(14) Uani 1 1 d .
H2A H 1.0193 0.2308 0.6221 0.105 Uiso 1 1 calc R
H2B H 0.9904 0.3143 0.5690 0.105 Uiso 1 1 calc R
H2C H 0.9032 0.1877 0.5701 0.105 Uiso 1 1 calc R
O11 O 0.76505(19) 0.11208(19) 0.7500 0.0313(8) Uani 1 2 d S
C12 C 0.7672(4) 0.0165(3) 0.7500 0.0551(16) Uani 1 2 d S
H12A H 0.7823 0.0020 0.8205 0.066 Uiso 0.50 1 calc PR
H12B H 0.8273 0.0252 0.7056 0.066 Uiso 0.50 1 calc PR
C13 C 0.6670(4) -0.0765(4) 0.7145(6) 0.047(4) Uani 0.50 1 d P
H13A H 0.6664 -0.0755 0.6386 0.057 Uiso 0.50 1 calc PR
H13B H 0.6667 -0.1432 0.7360 0.057 Uiso 0.50 1 calc PR
N14 N 0.5720(3) -0.0816(3) 0.7500 0.0331(10) Uani 1 2 d S
C14 C 0.5449(8) -0.1297(6) 0.8569(7) 0.070(3) Uani 0.50 1 d P
H14A H 0.6099 -0.0947 0.8999 0.104 Uiso 0.50 1 calc PR
H14B H 0.5187 -0.2076 0.8531 0.104 Uiso 0.50 1 calc PR
H14C H 0.4885 -0.1180 0.8867 0.104 Uiso 0.50 1 calc PR
C15 C 0.4808(5) -0.1308(5) 0.6866(7) 0.049(2) Uani 0.50 1 d P
H15A H 0.4464 -0.2104 0.6935 0.059 Uiso 0.50 1 calc PR
H15B H 0.5041 -0.1120 0.6144 0.059 Uiso 0.50 1 calc PR
C16 C 0.3987(4) -0.0978(4) 0.7106(5) 0.041(2) Uani 0.50 1 d P
H16A H 0.3453 -0.1205 0.6542 0.049 Uiso 0.50 1 calc PR
H16B H 0.3594 -0.1343 0.7742 0.049 Uiso 0.50 1 calc PR
O17 O 0.4497(2) 0.0150(2) 0.7234(5) 0.029(2) Uani 0.50 1 d P
O1L O 1.0000 0.0000 0.609(3) 0.066(10) Uani 0.13 3 d SP
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'
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Sn1 C1 170.92(17) . 10_557
C1 Sn1 O1 93.25(8) . 3_665
C1 Sn1 O1 93.25(8) 10_557 3_665
C1 Sn1 O1 92.70(9) . .
C1 Sn1 O1 92.70(9) 10_557 .
O1 Sn1 O1 97.70(12) 3_665 .
C1 Sn1 O11 87.40(8) . .
C1 Sn1 O11 87.40(8) 10_557 .
O1 Sn1 O11 169.29(9) 3_665 .
O1 Sn1 O11 71.59(9) . .
C1 Sn1 O17 79.50(18) . .
C1 Sn1 O17 96.63(18) 10_557 .
O1 Sn1 O17 71.18(10) 3_665 .
O1 Sn1 O17 165.81(12) . .
O11 Sn1 O17 119.39(9) . .
C1 Sn1 O17 96.63(18) . 10_557
C1 Sn1 O17 79.50(18) 10_557 10_557
O1 Sn1 O17 71.18(10) 3_665 10_557
O1 Sn1 O17 165.81(12) . 10_557
O11 Sn1 O17 119.39(9) . 10_557
O17 Sn1 O17 17.2(3) . 10_557
Sn2 O1 Sn1 109.16(11) . 2_655
Sn2 O1 Sn1 108.54(10) . .
Sn1 O1 Sn1 142.30(12) 2_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 . .
O1 Sn2 O11 79.21(10) . .
O1 Sn2 O17 78.29(11) . 11_657
O11 Sn2 O17 155.53(12) . 11_657
O1 Sn2 O17 78.29(11) . 2_655
O11 Sn2 O17 155.53(12) . 2_655
O17 Sn2 O17 19.0(3) 11_657 2_655
O1 Sn2 C2 119.63(11) . 10_557
O11 Sn2 C2 94.89(12) . 10_557
O17 Sn2 C2 87.95(19) 11_657 10_557
O17 Sn2 C2 104.53(19) 2_655 10_557
O1 Sn2 C2 119.63(11) . .
O11 Sn2 C2 94.89(12) . .
O17 Sn2 C2 104.53(19) 11_657 .
O17 Sn2 C2 87.95(19) 2_655 .
C2 Sn2 C2 120.7(2) 10_557 .
Sn2 C2 H2A 109.5 . .
Sn2 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Sn2 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C12 O11 Sn2 125.7(2) . .
C12 O11 Sn1 133.6(2) . .
Sn2 O11 Sn1 100.65(10) . .
O11 C12 C13 113.8(4) . .
O11 C12 H12A 108.8 . .
C13 C12 H12A 108.8 . .
O11 C12 H12B 108.8 . .
C13 C12 H12B 108.8 . .
H12A C12 H12B 107.7 . .
N14 C13 C12 115.2(5) . .
N14 C13 H13A 108.5 . .
C12 C13 H13A 108.5 . .
N14 C13 H13B 108.5 . .
C12 C13 H13B 108.5 . .
H13A C13 H13B 107.5 . .
C15 N14 C15 72.5(7) . 10_557
C15 N14 C13 148.8(4) . 10_557
C15 N14 C13 117.6(5) 10_557 10_557
C15 N14 C13 117.6(4) . .
C15 N14 C13 148.8(4) 10_557 .
C13 N14 C13 38.7(7) 10_557 .
C15 N14 C14 42.8(4) . 10_557
C15 N14 C14 110.7(6) 10_557 10_557
C13 N14 C14 110.4(5) 10_557 10_557
C13 N14 C14 74.9(5) . 10_557
C15 N14 C14 110.7(6) . .
C15 N14 C14 42.8(4) 10_557 .
C13 N14 C14 74.9(5) 10_557 .
C13 N14 C14 110.4(5) . .
C14 N14 C14 133.7(7) 10_557 .
N14 C14 H14A 109.5 . .
N14 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N14 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N14 C15 C16 113.3(6) . .
N14 C15 H15A 108.9 . .
C16 C15 H15A 108.9 . .
N14 C15 H15B 108.9 . .
C16 C15 H15B 108.9 . .
H15A C15 H15B 107.7 . .
O17 C16 C15 110.2(4) . .
O17 C16 C15 99.3(4) . 10_557
C15 C16 C15 54.6(6) . 10_557
O17 C16 H16A 109.6 . .
C15 C16 H16A 109.6 . .
C15 C16 H16A 150.9 10_557 .
O17 C16 H16B 109.6 . .
C15 C16 H16B 109.6 . .
C15 C16 H16B 63.6 10_557 .
H16A C16 H16B 108.1 . .
C16 O17 C16 38.5(5) . 10_557
C16 O17 Sn2 124.2(3) . 3_665
C16 O17 Sn2 112.2(3) 10_557 3_665
C16 O17 Sn1 135.0(3) . .
C16 O17 Sn1 120.8(3) 10_557 .
Sn2 O17 Sn1 100.03(13) 3_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C1 2.110(3) .
Sn1 C1 2.110(3) 10_557
Sn1 O1 2.145(2) 3_665
Sn1 O1 2.146(3) .
Sn1 O11 2.314(2) .
Sn1 O17 2.323(3) .
Sn1 O17 2.323(3) 10_557
O1 Sn2 2.020(2) .
O1 Sn1 2.145(2) 2_655
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
Sn2 O11 2.077(2) .
Sn2 O17 2.104(3) 11_657
Sn2 O17 2.104(3) 2_655
Sn2 C2 2.119(4) 10_557
Sn2 C2 2.119(4) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
O11 C12 1.378(5) .
C12 C13 1.456(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N14 1.399(6) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
N14 C15 1.399(7) .
N14 C15 1.399(7) 10_557
N14 C13 1.399(6) 10_557
N14 C14 1.517(8) 10_557
N14 C14 1.517(8) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.497(7) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 O17 1.406(6) .
C16 C15 1.985(10) 10_557
C16 H16A 0.9900 .
C16 H16B 0.9900 .
O17 C16 1.640(7) 10_557
O17 Sn2 2.104(3) 3_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 Sn1 O1 Sn2 -86.35(8) . .
C1 Sn1 O1 Sn2 86.35(8) 10_557 .
O1 Sn1 O1 Sn2 180.0 3_665 .
O11 Sn1 O1 Sn2 0.0 . .
O17 Sn1 O1 Sn2 -142.5(6) . .
O17 Sn1 O1 Sn2 142.5(6) 10_557 .
C1 Sn1 O1 Sn1 93.65(8) . 2_655
C1 Sn1 O1 Sn1 -93.65(8) 10_557 2_655
O1 Sn1 O1 Sn1 0.0 3_665 2_655
O11 Sn1 O1 Sn1 180.0 . 2_655
O17 Sn1 O1 Sn1 37.5(6) . 2_655
O17 Sn1 O1 Sn1 -37.5(6) 10_557 2_655
Sn1 O1 Sn2 O11 180.0 2_655 .
Sn1 O1 Sn2 O11 0.0 . .
Sn1 O1 Sn2 O17 9.69(18) 2_655 11_657
Sn1 O1 Sn2 O17 -170.31(18) . 11_657
Sn1 O1 Sn2 O17 -9.69(18) 2_655 2_655
Sn1 O1 Sn2 O17 170.31(18) . 2_655
Sn1 O1 Sn2 C2 90.49(13) 2_655 10_557
Sn1 O1 Sn2 C2 -89.51(13) . 10_557
Sn1 O1 Sn2 C2 -90.49(13) 2_655 .
Sn1 O1 Sn2 C2 89.51(13) . .
O1 Sn2 O11 C12 180.0 . .
O17 Sn2 O11 C12 -156.5(4) 11_657 .
O17 Sn2 O11 C12 156.5(4) 2_655 .
C2 Sn2 O11 C12 -60.74(10) 10_557 .
C2 Sn2 O11 C12 60.74(10) . .
O1 Sn2 O11 Sn1 0.0 . .
O17 Sn2 O11 Sn1 23.5(4) 11_657 .
O17 Sn2 O11 Sn1 -23.5(4) 2_655 .
C2 Sn2 O11 Sn1 119.26(10) 10_557 .
C2 Sn2 O11 Sn1 -119.26(10) . .
C1 Sn1 O11 C12 -86.28(9) . .
C1 Sn1 O11 C12 86.28(9) 10_557 .
O1 Sn1 O11 C12 180.0 3_665 .
O1 Sn1 O11 C12 180.0 . .
O17 Sn1 O11 C12 -9.87(18) . .
O17 Sn1 O11 C12 9.87(18) 10_557 .
C1 Sn1 O11 Sn2 93.72(9) . .
C1 Sn1 O11 Sn2 -93.72(9) 10_557 .
O1 Sn1 O11 Sn2 0.0 3_665 .
O1 Sn1 O11 Sn2 0.0 . .
O17 Sn1 O11 Sn2 170.13(18) . .
O17 Sn1 O11 Sn2 -170.13(18) 10_557 .
Sn2 O11 C12 C13 -159.6(3) . .
Sn1 O11 C12 C13 20.4(3) . .
O11 C12 C13 N14 -41.5(6) . .
C12 C13 N14 C15 149.5(5) . .
C12 C13 N14 C15 -108.4(9) . 10_557
C12 C13 N14 C13 -57.5(5) . 10_557
C12 C13 N14 C14 146.4(6) . 10_557
C12 C13 N14 C14 -82.1(6) . .
C15 N14 C15 C16 53.2(6) 10_557 .
C13 N14 C15 C16 167.9(7) 10_557 .
C13 N14 C15 C16 -158.9(5) . .
C14 N14 C15 C16 -154.4(10) 10_557 .
C14 N14 C15 C16 72.9(6) . .
N14 C15 C16 O17 45.8(8) . .
N14 C15 C16 C15 -41.3(5) . 10_557
C15 C16 O17 C16 -100.4(5) . 10_557
C15 C16 O17 C16 -44.9(3) 10_557 10_557
C15 C16 O17 Sn2 176.4(5) . 3_665
C15 C16 O17 Sn2 -128.0(4) 10_557 3_665
C15 C16 O17 Sn1 -15.8(10) . .
C15 C16 O17 Sn1 39.8(7) 10_557 .
C1 Sn1 O17 C16 84.8(7) . .
C1 Sn1 O17 C16 -86.9(7) 10_557 .
O1 Sn1 O17 C16 -178.1(7) 3_665 .
O1 Sn1 O17 C16 142.3(5) . .
O11 Sn1 O17 C16 3.8(7) . .
O17 Sn1 O17 C16 -91.1(7) 10_557 .
C1 Sn1 O17 C16 130.9(4) . 10_557
C1 Sn1 O17 C16 -40.8(4) 10_557 10_557
O1 Sn1 O17 C16 -132.0(4) 3_665 10_557
O1 Sn1 O17 C16 -171.6(4) . 10_557
O11 Sn1 O17 C16 50.0(4) . 10_557
O17 Sn1 O17 C16 -44.9(4) 10_557 10_557
C1 Sn1 O17 Sn2 -105.5(2) . 3_665
C1 Sn1 O17 Sn2 82.8(2) 10_557 3_665
O1 Sn1 O17 Sn2 -8.36(15) 3_665 3_665
O1 Sn1 O17 Sn2 -48.0(7) . 3_665
O11 Sn1 O17 Sn2 173.57(11) . 3_665
O17 Sn1 O17 Sn2 78.7(2) 10_557 3_665
