#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/56/7005695.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_7005695
loop_
_publ_author_name
'Dickie, Diane A.'
'Lee, Peter T. K.'
'Labeodan, Ojisamola A.'
'Schatte, Gabriele'
'Weinberg, Noham'
'Lewis, Andrew R.'
'Bernard, Guy M.'
'Wasylishen, Roderick E.'
'Clyburne, Jason A. C.'
_publ_section_title
;
 Flexible coordination of the carboxylate ligand in tin(II) amides and
 a 1,3-diaza-2,4-distannacyclobutanediyl.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2862
_journal_page_last               2869
_journal_paper_doi               10.1039/b704588c
_journal_year                    2007
_chemical_formula_sum            'C13 H38 Cl2 N2 Si4 Sn'
_chemical_formula_weight         524.40
_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                105.9710(12)
_cell_angle_beta                 96.8970(13)
_cell_angle_gamma                108.9690(14)
_cell_formula_units_Z            2
_cell_length_a                   8.55900(10)
_cell_length_b                   11.3010(2)
_cell_length_c                   14.9150(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1276.35(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10241
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  0.8178
_exptl_absorpt_correction_T_min  0.7674
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         6077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0247
_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)+(0.0168P)²+1.0619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                5637
_reflns_number_total             6077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704588c.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005695
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
Sn1 Sn 0.660437(16) 0.444566(13) 0.676384(9) 0.01975(4) Uani 1 1 d . . .
Cl1 Cl 0.40699(7) 0.46073(6) 0.60783(4) 0.03341(12) Uani 1 1 d . . .
Cl2 Cl 0.89580(8) 0.31199(7) 0.55721(5) 0.04357(14) Uani 1 1 d . . .
Si1 Si 0.40259(7) 0.15310(6) 0.66031(4) 0.02709(12) Uani 1 1 d . . .
Si2 Si 0.74804(7) 0.27366(6) 0.80546(4) 0.02450(12) Uani 1 1 d . . .
Si3 Si 0.67367(8) 0.67176(6) 0.86936(4) 0.02814(12) Uani 1 1 d . . .
Si4 Si 0.94925(8) 0.73847(6) 0.75618(4) 0.02794(13) Uani 1 1 d . . .
N1 N 0.5977(2) 0.28342(16) 0.72001(12) 0.0214(3) Uani 1 1 d . . .
N2 N 0.7790(2) 0.62411(16) 0.78056(12) 0.0245(3) Uani 1 1 d . . .
C1 C 0.7646(3) 0.4053(2) 0.55146(16) 0.0303(5) Uani 1 1 d . . .
H1A H 0.6703 0.3558 0.4937 0.036 Uiso 1 1 calc R . .
H1B H 0.8322 0.4908 0.5449 0.036 Uiso 1 1 calc R . .
C11 C 0.3718(4) 0.1160(2) 0.52807(17) 0.0414(6) Uani 1 1 d . . .
H11A H 0.3500 0.1880 0.5112 0.050 Uiso 1 1 calc R . .
H11B H 0.2749 0.0323 0.4951 0.050 Uiso 1 1 calc R . .
H11C H 0.4744 0.1082 0.5085 0.050 Uiso 1 1 calc R . .
C12 C 0.3908(3) -0.0042(2) 0.6827(2) 0.0420(6) Uani 1 1 d . . .
H12A H 0.4743 -0.0353 0.6549 0.050 Uiso 1 1 calc R . .
H12B H 0.2767 -0.0720 0.6531 0.050 Uiso 1 1 calc R . .
H12C H 0.4154 0.0123 0.7519 0.050 Uiso 1 1 calc R . .
C13 C 0.2208(3) 0.1909(3) 0.6999(2) 0.0496(7) Uani 1 1 d . . .
H13A H 0.2357 0.2084 0.7691 0.060 Uiso 1 1 calc R . .
H13B H 0.1148 0.1149 0.6661 0.060 Uiso 1 1 calc R . .
H13C H 0.2162 0.2693 0.6852 0.060 Uiso 1 1 calc R . .
C21 C 0.8047(3) 0.1252(2) 0.76076(19) 0.0373(5) Uani 1 1 d . . .
H21A H 0.7155 0.0466 0.7635 0.045 Uiso 1 1 calc R . .
H21B H 0.9128 0.1391 0.8009 0.045 Uiso 1 1 calc R . .
H21C H 0.8154 0.1120 0.6944 0.045 Uiso 1 1 calc R . .
C22 C 0.6687(4) 0.2690(3) 0.91593(19) 0.0510(7) Uani 1 1 d . . .
H22A H 0.6578 0.3536 0.9467 0.061 Uiso 1 1 calc R . .
H22B H 0.7490 0.2545 0.9603 0.061 Uiso 1 1 calc R . .
H22C H 0.5577 0.1966 0.8989 0.061 Uiso 1 1 calc R . .
C23 C 0.9524(3) 0.4194(2) 0.8379(2) 0.0438(6) Uani 1 1 d . . .
H23A H 0.9948 0.4228 0.7801 0.053 Uiso 1 1 calc R . .
H23B H 1.0361 0.4106 0.8840 0.053 Uiso 1 1 calc R . .
H23C H 0.9335 0.5012 0.8667 0.053 Uiso 1 1 calc R . .
C31 C 0.4760(3) 0.5322(3) 0.86124(19) 0.0406(6) Uani 1 1 d . . .
H31A H 0.3928 0.5114 0.8024 0.049 Uiso 1 1 calc R . .
H31B H 0.4287 0.5580 0.9168 0.049 Uiso 1 1 calc R . .
H31C H 0.5024 0.4538 0.8602 0.049 Uiso 1 1 calc R . .
C32 C 0.8108(4) 0.7224(3) 0.99114(18) 0.0499(7) Uani 1 1 d . . .
H32A H 0.8393 0.6477 0.9982 0.060 Uiso 1 1 calc R . .
H32B H 0.7497 0.7484 1.0398 0.060 Uiso 1 1 calc R . .
H32C H 0.9153 0.7976 0.9993 0.060 Uiso 1 1 calc R . .
C33 C 0.6091(4) 0.8110(3) 0.8581(2) 0.0464(6) Uani 1 1 d . . .
H33A H 0.7107 0.8908 0.8713 0.056 Uiso 1 1 calc R . .
H33B H 0.5400 0.8287 0.9041 0.056 Uiso 1 1 calc R . .
H33C H 0.5428 0.7863 0.7929 0.056 Uiso 1 1 calc R . .
C41 C 1.1137(3) 0.6692(3) 0.7254(2) 0.0440(6) Uani 1 1 d . . .
H41A H 1.1663 0.6548 0.7815 0.053 Uiso 1 1 calc R . .
H41B H 1.2007 0.7318 0.7060 0.053 Uiso 1 1 calc R . .
H41C H 1.0604 0.5844 0.6726 0.053 Uiso 1 1 calc R . .
C42 C 1.0616(4) 0.8916(3) 0.8629(2) 0.0513(7) Uani 1 1 d . . .
H42A H 0.9808 0.9322 0.8833 0.062 Uiso 1 1 calc R . .
H42B H 1.1525 0.9547 0.8462 0.062 Uiso 1 1 calc R . .
H42C H 1.1104 0.8683 0.9153 0.062 Uiso 1 1 calc R . .
C43 C 0.8681(3) 0.7865(2) 0.65562(18) 0.0372(5) Uani 1 1 d . . .
H43A H 0.8079 0.7068 0.5993 0.045 Uiso 1 1 calc R . .
H43B H 0.9636 0.8472 0.6401 0.045 Uiso 1 1 calc R . .
H43C H 0.7901 0.8308 0.6746 0.045 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'
Cl Cl 0.1484 0.1585 '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'
Si Si 0.0817 0.0704 '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
N2 Sn1 N1 116.50(7) . . ?
N2 Sn1 C1 117.81(8) . . ?
N1 Sn1 C1 109.66(8) . . ?
N2 Sn1 Cl1 102.34(5) . . ?
N1 Sn1 Cl1 108.49(5) . . ?
C1 Sn1 Cl1 99.94(6) . . ?
N1 Si1 C13 112.08(11) . . ?
N1 Si1 C11 110.28(10) . . ?
C13 Si1 C11 109.47(14) . . ?
N1 Si1 C12 112.06(10) . . ?
C13 Si1 C12 106.21(13) . . ?
C11 Si1 C12 106.51(12) . . ?
N1 Si2 C22 110.58(11) . . ?
N1 Si2 C21 112.96(10) . . ?
C22 Si2 C21 108.46(13) . . ?
N1 Si2 C23 110.64(9) . . ?
C22 Si2 C23 108.93(15) . . ?
C21 Si2 C23 105.06(12) . . ?
N2 Si3 C31 111.53(10) . . ?
N2 Si3 C32 110.62(12) . . ?
C31 Si3 C32 106.66(13) . . ?
N2 Si3 C33 111.53(11) . . ?
C31 Si3 C33 106.77(13) . . ?
C32 Si3 C33 109.53(14) . . ?
N2 Si4 C43 109.43(10) . . ?
N2 Si4 C41 111.70(10) . . ?
C43 Si4 C41 109.85(13) . . ?
N2 Si4 C42 111.55(11) . . ?
C43 Si4 C42 108.65(13) . . ?
C41 Si4 C42 105.56(14) . . ?
Si2 N1 Si1 123.22(9) . . ?
Si2 N1 Sn1 118.94(9) . . ?
Si1 N1 Sn1 117.49(9) . . ?
Si3 N2 Si4 122.74(10) . . ?
Si3 N2 Sn1 118.44(9) . . ?
Si4 N2 Sn1 116.17(9) . . ?
Cl2 C1 Sn1 112.76(11) . . ?
Cl2 C1 H1A 109.0 . . ?
Sn1 C1 H1A 109.0 . . ?
Cl2 C1 H1B 109.0 . . ?
Sn1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si3 C31 H31A 109.5 . . ?
Si3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si3 C32 H32A 109.5 . . ?
Si3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si3 C33 H33A 109.5 . . ?
Si3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si4 C41 H41A 109.5 . . ?
Si4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si4 C42 H42A 109.5 . . ?
Si4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si4 C43 H43A 109.5 . . ?
Si4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
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
Sn1 N2 2.0270(17) . ?
Sn1 N1 2.0318(16) . ?
Sn1 C1 2.160(2) . ?
Sn1 Cl1 2.3689(5) . ?
Cl2 C1 1.782(2) . ?
Si1 N1 1.7530(17) . ?
Si1 C13 1.862(3) . ?
Si1 C11 1.867(3) . ?
Si1 C12 1.871(3) . ?
Si2 N1 1.7516(17) . ?
Si2 C22 1.863(3) . ?
Si2 C21 1.867(2) . ?
Si2 C23 1.869(3) . ?
Si3 N2 1.7508(19) . ?
Si3 C31 1.864(3) . ?
Si3 C32 1.866(3) . ?
Si3 C33 1.870(3) . ?
Si4 N2 1.7574(18) . ?
Si4 C43 1.863(2) . ?
Si4 C41 1.865(3) . ?
Si4 C42 1.868(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 Si2 N1 Si1 -68.63(16) . . . . ?
C21 Si2 N1 Si1 53.13(15) . . . . ?
C23 Si2 N1 Si1 170.59(13) . . . . ?
C22 Si2 N1 Sn1 118.31(14) . . . . ?
C21 Si2 N1 Sn1 -119.93(11) . . . . ?
C23 Si2 N1 Sn1 -2.47(15) . . . . ?
C13 Si1 N1 Si2 109.54(15) . . . . ?
C11 Si1 N1 Si2 -128.23(13) . . . . ?
C12 Si1 N1 Si2 -9.77(16) . . . . ?
C13 Si1 N1 Sn1 -77.31(14) . . . . ?
C11 Si1 N1 Sn1 44.93(14) . . . . ?
C12 Si1 N1 Sn1 163.39(11) . . . . ?
N2 Sn1 N1 Si2 -45.29(12) . . . . ?
C1 Sn1 N1 Si2 91.73(11) . . . . ?
Cl1 Sn1 N1 Si2 -160.04(8) . . . . ?
N2 Sn1 N1 Si1 141.25(9) . . . . ?
C1 Sn1 N1 Si1 -81.73(11) . . . . ?
Cl1 Sn1 N1 Si1 26.51(10) . . . . ?
C31 Si3 N2 Si4 169.37(13) . . . . ?
C32 Si3 N2 Si4 -72.09(15) . . . . ?
C33 Si3 N2 Si4 50.08(16) . . . . ?
C31 Si3 N2 Sn1 8.54(15) . . . . ?
C32 Si3 N2 Sn1 127.08(13) . . . . ?
C33 Si3 N2 Sn1 -110.75(13) . . . . ?
C43 Si4 N2 Si3 -95.06(14) . . . . ?
C41 Si4 N2 Si3 143.07(14) . . . . ?
C42 Si4 N2 Si3 25.19(17) . . . . ?
C43 Si4 N2 Sn1 66.17(13) . . . . ?
C41 Si4 N2 Sn1 -55.69(14) . . . . ?
C42 Si4 N2 Sn1 -173.58(12) . . . . ?
N1 Sn1 N2 Si3 -59.89(12) . . . . ?
C1 Sn1 N2 Si3 166.65(9) . . . . ?
Cl1 Sn1 N2 Si3 58.27(10) . . . . ?
N1 Sn1 N2 Si4 138.04(9) . . . . ?
C1 Sn1 N2 Si4 4.57(13) . . . . ?
Cl1 Sn1 N2 Si4 -103.80(9) . . . . ?
N2 Sn1 C1 Cl2 98.30(12) . . . . ?
N1 Sn1 C1 Cl2 -38.10(14) . . . . ?
Cl1 Sn1 C1 Cl2 -151.96(10) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652691
