#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014257.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_7014257
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Hu, Jin'
'Lappert, Michael F.'
'Severn, John R.'
_publ_section_title
;
 Synthesis and structures of beta-diketiminatotin(II) halides, an amide
 and of Sn(=E)[{N(R)C(Ph)}2CH](NR2) (E = S or Se, R = SiMe3).
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4193
_journal_page_last               4201
_journal_paper_doi               10.1039/b412765j
_journal_year                    2004
_chemical_formula_moiety         '2(C13 H17 Cl N2 Sn), (C7 H8)'
_chemical_formula_sum            'C33 H42 Cl2 N4 Sn2'
_chemical_formula_weight         802.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.280(6)
_cell_length_b                   25.044(12)
_cell_length_c                   12.767(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3446(3)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'Nonius CAD4 software'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4776
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1037P)²+10.1016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                3434
_reflns_number_total             4776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412765j.txt
_cod_data_source_block           (6)-sep1096
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7014257
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.16112(8) 0.55651(3) 0.09960(6) 0.0299(3) Uani 1 1 d . . .
Cl1 Cl 0.0050(3) 0.50562(11) 0.1714(2) 0.0349(7) Uani 1 1 d . . .
N1 N 0.0097(9) 0.5994(4) -0.0087(7) 0.029(2) Uani 1 1 d . . .
H1 H -0.0142 0.5875 -0.0766 0.035 Uiso 1 1 calc R . .
N2 N 0.1710(9) 0.6246(4) 0.2015(8) 0.033(2) Uani 1 1 d . . .
H2 H 0.2363 0.6258 0.2599 0.039 Uiso 1 1 calc R . .
Sn2 Sn 0.29428(9) 0.48740(3) 0.42693(7) 0.0344(3) Uani 1 1 d . . .
Cl2 Cl 0.4089(3) 0.57374(13) 0.4051(3) 0.0456(9) Uani 1 1 d . . .
N3 N 0.3398(10) 0.4963(4) 0.5980(7) 0.033(2) Uani 1 1 d . . .
H3 H 0.3993 0.4748 0.6351 0.039 Uiso 1 1 calc R . .
N4 N 0.1343(9) 0.5302(4) 0.4345(8) 0.031(2) Uani 1 1 d . . .
H4 H 0.0711 0.5282 0.3745 0.037 Uiso 1 1 calc R . .
C1 C -0.0533(11) 0.6405(4) 0.0099(8) 0.027(3) Uani 1 1 d . . .
C2 C -0.0127(12) 0.6714(5) 0.1036(9) 0.031(3) Uani 1 1 d . . .
H2A H -0.0653 0.7003 0.1085 0.037 Uiso 1 1 calc R . .
C3 C 0.0929(10) 0.6662(4) 0.1904(8) 0.024(3) Uani 1 1 d . . .
C4 C -0.1791(12) 0.6545(5) -0.0747(9) 0.030(3) Uani 1 1 d . . .
C5 C -0.2055(13) 0.6197(5) -0.1753(10) 0.047(4) Uani 1 1 d . . .
H5A H -0.1414 0.6255 -0.2118 0.071 Uiso 1 1 calc R . .
H5B H -0.2869 0.6290 -0.2256 0.071 Uiso 1 1 calc R . .
H5C H -0.2052 0.5822 -0.1539 0.071 Uiso 1 1 calc R . .
C6 C -0.1814(16) 0.7131(6) -0.1068(14) 0.070(5) Uani 1 1 d . . .
H6A H -0.1160 0.7198 -0.1414 0.104 Uiso 1 1 calc R . .
H6B H -0.1672 0.7354 -0.0411 0.104 Uiso 1 1 calc R . .
H6C H -0.2623 0.7218 -0.1585 0.104 Uiso 1 1 calc R . .
C7 C -0.2783(13) 0.6443(7) -0.0221(11) 0.055(4) Uani 1 1 d . . .
H7A H -0.2637 0.6664 0.0438 0.082 Uiso 1 1 calc R . .
H7B H -0.2775 0.6065 -0.0020 0.082 Uiso 1 1 calc R . .
H7C H -0.3592 0.6533 -0.0736 0.082 Uiso 1 1 calc R . .
C8 C 0.1235(11) 0.7088(5) 0.2762(9) 0.030(3) Uani 1 1 d . . .
C9 C 0.1762(12) 0.6955(5) 0.3866(10) 0.037(3) Uani 1 1 d . . .
H9 H 0.1931 0.6592 0.4074 0.044 Uiso 1 1 calc R . .
C10 C 0.2036(11) 0.7353(5) 0.4653(10) 0.037(3) Uani 1 1 d . . .
H10 H 0.2383 0.7263 0.5404 0.044 Uiso 1 1 calc R . .
C11 C 0.1805(12) 0.7885(5) 0.4346(11) 0.042(3) Uani 1 1 d . . .
H11 H 0.2002 0.8157 0.4888 0.050 Uiso 1 1 calc R . .
C12 C 0.1283(14) 0.8019(5) 0.3244(11) 0.046(4) Uani 1 1 d . . .
H12 H 0.1126 0.8381 0.3026 0.056 Uiso 1 1 calc R . .
C13 C 0.1004(13) 0.7615(4) 0.2483(10) 0.037(3) Uani 1 1 d . . .
H13 H 0.0637 0.7705 0.1733 0.044 Uiso 1 1 calc R . .
C14 C 0.2949(11) 0.5286(5) 0.6611(10) 0.030(3) Uani 1 1 d . . .
C15 C 0.1961(12) 0.5592(5) 0.6195(10) 0.035(3) Uani 1 1 d . . .
H15 H 0.1795 0.5847 0.6685 0.042 Uiso 1 1 calc R . .
C16 C 0.1130(11) 0.5593(4) 0.5137(9) 0.029(3) Uani 1 1 d . . .
C17 C 0.3650(12) 0.5268(5) 0.7850(10) 0.038(3) Uani 1 1 d . . .
C18 C 0.3200(15) 0.5690(6) 0.8496(11) 0.053(4) Uani 1 1 d . . .
H18A H 0.2299 0.5661 0.8341 0.079 Uiso 1 1 calc R . .
H18B H 0.3410 0.6045 0.8282 0.079 Uiso 1 1 calc R . .
H18C H 0.3601 0.5636 0.9281 0.079 Uiso 1 1 calc R . .
C19 C 0.5017(13) 0.5317(7) 0.8090(11) 0.062(4) Uani 1 1 d . . .
H19A H 0.5315 0.5047 0.7674 0.093 Uiso 1 1 calc R . .
H19B H 0.5415 0.5264 0.8876 0.093 Uiso 1 1 calc R . .
H19C H 0.5221 0.5674 0.7877 0.093 Uiso 1 1 calc R . .
C20 C 0.3400(16) 0.4709(6) 0.8274(12) 0.065(5) Uani 1 1 d . . .
H20A H 0.2505 0.4660 0.8135 0.097 Uiso 1 1 calc R . .
H20B H 0.3816 0.4684 0.9064 0.097 Uiso 1 1 calc R . .
H20C H 0.3722 0.4431 0.7891 0.097 Uiso 1 1 calc R . .
C21 C -0.0020(11) 0.5917(4) 0.4859(9) 0.029(3) Uani 1 1 d . . .
C22 C -0.0575(12) 0.6084(5) 0.3798(10) 0.036(3) Uani 1 1 d . . .
H22 H -0.0202 0.5993 0.3244 0.044 Uiso 1 1 calc R . .
C23 C -0.1678(14) 0.6385(5) 0.3512(11) 0.046(4) Uani 1 1 d . . .
H23 H -0.2058 0.6491 0.2774 0.055 Uiso 1 1 calc R . .
C24 C -0.2191(12) 0.6521(5) 0.4317(11) 0.042(3) Uani 1 1 d . . .
H24 H -0.2938 0.6723 0.4140 0.051 Uiso 1 1 calc R . .
C25 C -0.1647(13) 0.6372(5) 0.5355(11) 0.044(4) Uani 1 1 d . . .
H25 H -0.2014 0.6482 0.5901 0.053 Uiso 1 1 calc R . .
C26 C -0.0589(13) 0.6070(5) 0.5670(10) 0.039(3) Uani 1 1 d . . .
H26 H -0.0243 0.5965 0.6413 0.046 Uiso 1 1 calc R . .
C27 C 0.4954(12) 0.7870(5) 0.6647(11) 0.071(5) Uani 1 1 d G . .
C28 C 0.4464(13) 0.7670(9) 0.7446(10) 0.147(13) Uani 1 1 d G . .
H28 H 0.4247 0.7906 0.7941 0.176 Uiso 1 1 calc R . .
C29 C 0.4291(13) 0.7123(10) 0.7521(14) 0.177(19) Uani 1 1 d G . .
H29 H 0.3956 0.6986 0.8067 0.213 Uiso 1 1 calc R . .
C30 C 0.4609(16) 0.6777(6) 0.6796(19) 0.31(4) Uani 1 1 d G . .
H30 H 0.4491 0.6403 0.6847 0.366 Uiso 1 1 calc R . .
C31 C 0.5099(15) 0.6977(6) 0.5997(15) 0.145(12) Uani 1 1 d G . .
H31 H 0.5316 0.6740 0.5502 0.174 Uiso 1 1 calc R . .
C32 C 0.5272(11) 0.7524(6) 0.5922(10) 0.082(6) Uani 1 1 d G . .
H32 H 0.5607 0.7661 0.5376 0.098 Uiso 1 1 calc R . .
C33 C 0.501(2) 0.8408(9) 0.654(3) 0.174(15) Uani 1 1 d . . .
H33A H 0.5374 0.8492 0.5951 0.260 Uiso 0.50 1 calc PR . .
H33B H 0.5534 0.8561 0.7231 0.260 Uiso 0.50 1 calc PR . .
H33C H 0.4177 0.8559 0.6368 0.260 Uiso 0.50 1 calc PR . .
H33D H 0.4683 0.8583 0.7082 0.260 Uiso 0.50 1 calc PR . .
H33E H 0.4523 0.8514 0.5802 0.260 Uiso 0.50 1 calc PR . .
H33F H 0.5880 0.8516 0.6665 0.260 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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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 83.1(3) . . ?
N2 Sn1 Cl1 95.6(3) . . ?
N1 Sn1 Cl1 88.8(3) . . ?
C1 N1 Sn1 130.4(7) . . ?
C3 N2 Sn1 129.9(8) . . ?
N3 Sn2 N4 81.3(4) . . ?
N3 Sn2 Cl2 92.7(3) . . ?
N4 Sn2 Cl2 92.4(3) . . ?
C14 N3 Sn2 131.9(8) . . ?
C16 N4 Sn2 131.3(8) . . ?
N1 C1 C2 122.5(11) . . ?
N1 C1 C4 119.0(9) . . ?
C2 C1 C4 118.5(10) . . ?
C3 C2 C1 129.1(11) . . ?
N2 C3 C2 123.0(10) . . ?
N2 C3 C8 118.2(10) . . ?
C2 C3 C8 118.8(10) . . ?
C7 C4 C5 107.5(12) . . ?
C7 C4 C6 109.4(12) . . ?
C5 C4 C6 110.1(11) . . ?
C7 C4 C1 107.7(10) . . ?
C5 C4 C1 112.0(10) . . ?
C6 C4 C1 110.1(10) . . ?
C13 C8 C9 118.9(11) . . ?
C13 C8 C3 120.7(11) . . ?
C9 C8 C3 120.3(11) . . ?
C10 C9 C8 119.8(12) . . ?
C9 C10 C11 120.2(12) . . ?
C10 C11 C12 120.1(11) . . ?
C13 C12 C11 118.5(13) . . ?
C12 C13 C8 122.5(12) . . ?
C15 C14 N3 122.0(12) . . ?
C15 C14 C17 122.8(11) . . ?
N3 C14 C17 115.3(11) . . ?
C14 C15 C16 129.1(11) . . ?
N4 C16 C15 121.1(11) . . ?
N4 C16 C21 117.5(10) . . ?
C15 C16 C21 121.4(10) . . ?
C19 C17 C18 108.9(12) . . ?
C19 C17 C14 113.3(10) . . ?
C18 C17 C14 112.6(11) . . ?
C19 C17 C20 106.6(13) . . ?
C18 C17 C20 108.2(12) . . ?
C14 C17 C20 106.9(11) . . ?
C22 C21 C26 117.6(11) . . ?
C22 C21 C16 120.8(11) . . ?
C26 C21 C16 121.6(10) . . ?
C21 C22 C23 121.7(12) . . ?
C24 C23 C22 118.6(12) . . ?
C25 C24 C23 120.3(13) . . ?
C24 C25 C26 123.4(13) . . ?
C25 C26 C21 118.4(12) . . ?
C33 C27 C28 118.2(19) . . ?
C33 C27 C32 121.6(19) . . ?
C28 C27 C32 120.0 . . ?
C27 C28 C29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C29 C30 C31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C31 C32 C27 120.0 . . ?
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 2.129(9) . ?
Sn1 N1 2.142(9) . ?
Sn1 Cl1 2.554(3) . ?
N1 C1 1.312(14) . ?
N2 C3 1.344(14) . ?
Sn2 N3 2.102(9) . ?
Sn2 N4 2.125(10) . ?
Sn2 Cl2 2.576(4) . ?
N3 C14 1.343(15) . ?
N4 C16 1.325(14) . ?
C1 C2 1.384(15) . ?
C1 C4 1.548(16) . ?
C2 C3 1.372(16) . ?
C3 C8 1.495(15) . ?
C4 C7 1.487(18) . ?
C4 C5 1.506(16) . ?
C4 C6 1.522(18) . ?
C8 C13 1.373(17) . ?
C8 C9 1.398(16) . ?
C9 C10 1.384(17) . ?
C10 C11 1.391(18) . ?
C11 C12 1.397(19) . ?
C12 C13 1.372(17) . ?
C14 C15 1.328(17) . ?
C14 C17 1.546(17) . ?
C15 C16 1.398(17) . ?
C16 C21 1.483(16) . ?
C17 C19 1.485(19) . ?
C17 C18 1.516(18) . ?
C17 C20 1.558(19) . ?
C21 C22 1.378(16) . ?
C21 C26 1.423(16) . ?
C22 C23 1.408(18) . ?
C23 C24 1.363(18) . ?
C24 C25 1.338(18) . ?
C25 C26 1.369(18) . ?
C27 C33 1.36(2) . ?
C27 C28 1.3900 . ?
C27 C32 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
