#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/83/4078374.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_4078374
loop_
_publ_author_name
'Willem, Rudolph'
'Bouhdid, Abdeslam'
'Meddour, Abdelkrim'
'Camacho-Camacho, Carlos'
'Mercier, Frédéric'
'Gielen, Marcel'
'Biesemans, Monique'
'Ribot, François'
'Sanchez, Clément'
'Tiekink, Edward R. T.'
_publ_section_title
;
 X-ray Diffraction and 2D Gradient-Assisted1H−119Sn HMQC NMR
 Studies of Structures Obtained from Nucleophilic Substitutions on
 Dimethyltin(IV) Salicylaldoximates
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4377
_journal_paper_doi               10.1021/om970378e
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C30 H38 N3 O6 Sn3'
_chemical_formula_weight         892.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Jan 10 13:23:19 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                103.00(3)
_cell_angle_beta                 102.90(2)
_cell_angle_gamma                86.63(4)
_cell_formula_units_Z            2
_cell_length_a                   12.334(5)
_cell_length_b                   14.624(7)
_cell_length_c                   10.101(3)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293
_cell_measurement_theta_max      46.9
_cell_measurement_theta_min      43.6
_cell_volume                     1730.4(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.01358
_diffrn_orient_matrix_UB_12      -0.00018
_diffrn_orient_matrix_UB_13      -0.10157
_diffrn_orient_matrix_UB_21      0.07776
_diffrn_orient_matrix_UB_22      -0.02334
_diffrn_orient_matrix_UB_23      -0.00149
_diffrn_orient_matrix_UB_31      -0.02634
_diffrn_orient_matrix_UB_32      -0.06631
_diffrn_orient_matrix_UB_33      -0.02350
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  17.19
_diffrn_reflns_av_sigmaI/netI    12.8
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8339
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -19.34
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             874.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.660
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4821
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.0039
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0391
_reflns_number_observed          4821
_reflns_number_total             7972
_reflns_observed_criterion       3.00
_cod_data_source_file            om970378e.cif
_cod_data_source_block           4
_cod_original_cell_volume        1730(1)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C30 H38 N3 O6 Sn3 '
_cod_database_code               4078374
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Sn(1) 0.04531(4) 0.29676(3) 0.05456(4) 0.0456(1) Uij
Sn(2) -0.19128(4) 0.18227(3) 0.09972(4) 0.0486(1) Uij
Sn(3) -0.09703(4) 0.37036(3) 0.35364(4) 0.0489(1) Uij
O(9) 0.1735(4) 0.2219(4) -0.2141(4) 0.078(2) Uij
O(10) -0.1033(3) 0.1566(3) -0.0669(4) 0.050(1) Uij
O(19) 0.0171(4) 0.4584(3) 0.3222(5) 0.071(2) Uij
O(20) 0.1914(4) 0.3511(4) 0.0115(5) 0.082(2) Uij
O(30) -0.0787(3) 0.2847(3) 0.1729(4) 0.049(1) Uij
O(40) -0.2154(4) 0.2508(3) 0.3116(5) 0.071(2) Uij
N(4) -0.3224(6) 0.2639(5) 0.3392(6) 0.076(2) Uij
N(8) 0.0737(5) 0.1978(4) -0.1870(5) 0.058(2) Uij
N(18) 0.0945(4) 0.4237(4) 0.2421(5) 0.051(2) Uij
C(1) -0.0863(6) 0.0976(4) -0.3011(6) 0.048(2) Uij
C(2) -0.1401(5) 0.1006(4) -0.1912(6) 0.045(2) Uij
C(3) -0.2312(6) 0.0424(5) -0.2171(6) 0.059(2) Uij
C(4) -0.2728(7) -0.0143(5) -0.3472(8) 0.073(3) Uij
C(5) -0.2238(7) -0.0146(5) -0.4571(7) 0.074(3) Uij
C(6) -0.1311(7) 0.0408(5) -0.4322(6) 0.065(2) Uij
C(7) 0.0164(6) 0.1422(5) -0.2919(6) 0.058(2) Uij
C(11) 0.2777(5) 0.4603(4) 0.2139(7) 0.052(2) Uij
C(12) 0.2794(6) 0.3977(5) 0.0867(7) 0.059(2) Uij
C(13) 0.3779(7) 0.3884(5) 0.0393(8) 0.074(3) Uij
C(14) 0.4690(7) 0.4419(6) 0.1134(10) 0.086(3) Uij
C(15) 0.4667(7) 0.5058(6) 0.2371(10) 0.087(3) Uij
C(16) 0.3710(6) 0.5134(5) 0.2844(8) 0.072(3) Uij
C(17) 0.1826(6) 0.4738(4) 0.2769(6) 0.054(2) Uij
C(21) -0.0656(6) 0.3732(4) -0.0733(7) 0.065(2) Uij
C(22) 0.1408(6) 0.1895(5) 0.1377(7) 0.070(2) Uij
C(23) -0.1372(7) 0.0565(5) 0.1665(7) 0.075(3) Uij
C(24) -0.3434(6) 0.2291(6) -0.0071(8) 0.081(3) Uij
C(25) 0.0028(7) 0.3171(6) 0.5204(8) 0.090(3) Uij
C(26) -0.2247(6) 0.4729(5) 0.3356(8) 0.078(3) Uij
C(41) -0.3378(7) 0.2330(5) 0.4354(8) 0.075(3) Uij
C(42) -0.4451(6) 0.2416(5) 0.4788(7) 0.060(2) Uij
C(43) -0.5374(7) 0.2870(5) 0.4163(8) 0.074(3) Uij
C(44) -0.6313(7) 0.2939(6) 0.4660(9) 0.080(3) Uij
C(45) -0.6402(7) 0.2554(6) 0.5743(9) 0.077(3) Uij
C(46) -0.5510(8) 0.2086(7) 0.6349(8) 0.090(3) Uij
C(47) -0.4536(7) 0.2014(6) 0.5888(9) 0.090(3) Uij
C(101) 0.5812(9) -0.0580(10) 0.054(2) 0.128(5) Uij
C(102) 0.540(1) -0.0735(9) -0.087(2) 0.127(6) Uij
C(103) 0.459(1) -0.016(1) -0.142(1) 0.127(5) Uij
H(3) -0.2671 0.0412 -0.1413 0.0708 Uij
H(4) -0.3366 -0.0538 -0.3605 0.0874 Uij
H(5) -0.2533 -0.0525 -0.5489 0.0888 Uij
H(6) -0.0953 0.0404 -0.5087 0.0778 Uij
H(7) 0.0460 0.1284 -0.3756 0.0695 Uij
H(9) 0.2194 0.2648 -0.1308 0.0767 Uij
H(13) 0.3825 0.3439 -0.0464 0.0882 Uij
H(14) 0.5367 0.4347 0.0780 0.1034 Uij
H(15) 0.5310 0.5436 0.2880 0.1048 Uij
H(16) 0.3677 0.5578 0.3707 0.0868 Uij
H(17) 0.1854 0.5270 0.3547 0.0645 Uij
H(21b) -0.0286 0.3890 -0.1403 0.0777 Uij
H(21c) -0.1303 0.3353 -0.1220 0.0777 Uij
H(21a) -0.0886 0.4303 -0.0161 0.0777 Uij
H(22b) 0.2086 0.1789 0.1026 0.0835 Uij
H(22c) 0.1595 0.2085 0.2384 0.0835 Uij
H(22a) 0.0982 0.1321 0.1100 0.0835 Uij
H(23b) -0.1187 0.0102 0.0895 0.0902 Uij
H(23c) -0.0720 0.0691 0.2419 0.0902 Uij
H(23a) -0.1962 0.0328 0.1987 0.0902 Uij
H(24b) -0.3512 0.2049 -0.1063 0.0969 Uij
H(24c) -0.4042 0.2068 0.0234 0.0969 Uij
H(24a) -0.3448 0.2972 0.0125 0.0969 Uij
H(25b) 0.0279 0.2541 0.4851 0.1082 Uij
H(25c) 0.0667 0.3573 0.5633 0.1082 Uij
H(25a) -0.0407 0.3157 0.5890 0.1082 Uij
H(26b) -0.2362 0.4883 0.2449 0.0930 Uij
H(26c) -0.2930 0.4485 0.3461 0.0930 Uij
H(26a) -0.2034 0.5289 0.4076 0.0930 Uij
H(41) -0.2766 0.2012 0.4860 0.0903 Uij
H(43) -0.5348 0.3136 0.3374 0.0888 Uij
H(44) -0.6948 0.3274 0.4232 0.0954 Uij
H(45) -0.7088 0.2613 0.6075 0.0923 Uij
H(46) -0.5563 0.1801 0.7112 0.1074 Uij
H(47) -0.3903 0.1681 0.6329 0.1077 Uij
H(101) 0.6385 -0.0992 0.0924 0.1533 Uij
H(102) 0.5681 -0.1255 -0.1489 0.1528 Uij
H(103) 0.4297 -0.0270 -0.2415 0.1520 Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 60 0.003 0.002 'International Tables'
H 0 76 0.000 0.000 'International Tables'
N 0 6 0.006 0.003 'International Tables'
O 0 12 0.011 0.006 'International Tables'
Sn 0 6 -0.654 1.425 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 -2 -1
-2 2 -1
3 0 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(10) Sn(1) O(20) 137.6(1) yes
O(10) Sn(1) O(30) 65.3(1) yes
O(10) Sn(1) N(8) 65.1(1) yes
O(10) Sn(1) N(18) 145.0(1) yes
O(10) Sn(1) C(21) 83.5(2) yes
O(10) Sn(1) C(22) 83.3(2) yes
O(20) Sn(1) O(30) 157.1(2) yes
O(20) Sn(1) N(8) 72.5(2) yes
O(20) Sn(1) N(18) 77.4(2) yes
O(20) Sn(1) C(21) 92.9(2) yes
O(20) Sn(1) C(22) 91.6(3) yes
O(30) Sn(1) N(8) 130.3(2) yes
O(30) Sn(1) N(18) 79.8(2) yes
O(30) Sn(1) C(21) 92.0(2) yes
O(30) Sn(1) C(22) 89.6(2) yes
N(8) Sn(1) N(18) 149.7(2) yes
N(8) Sn(1) C(21) 82.3(2) yes
N(8) Sn(1) C(22) 85.0(2) yes
N(18) Sn(1) C(21) 95.7(2) yes
N(18) Sn(1) C(22) 99.6(2) yes
C(21) Sn(1) C(22) 164.6(3) yes
O(10) Sn(2) O(30) 80.1(1) yes
O(10) Sn(2) O(40) 153.8(2) yes
O(10) Sn(2) C(23) 95.1(2) yes
O(10) Sn(2) C(24) 98.5(2) yes
O(30) Sn(2) O(40) 74.1(2) yes
O(30) Sn(2) C(23) 113.0(3) yes
O(30) Sn(2) C(24) 112.2(3) yes
O(40) Sn(2) C(23) 90.8(2) yes
O(40) Sn(2) C(24) 95.5(2) yes
C(23) Sn(2) C(24) 134.3(3) yes
O(19) Sn(3) O(30) 86.9(2) yes
O(19) Sn(3) O(40) 159.9(2) yes
O(19) Sn(3) C(25) 99.9(3) yes
O(19) Sn(3) C(26) 91.5(3) yes
O(30) Sn(3) O(40) 73.3(2) yes
O(30) Sn(3) C(25) 108.4(2) yes
O(30) Sn(3) C(26) 115.4(2) yes
O(40) Sn(3) C(25) 89.5(3) yes
O(40) Sn(3) C(26) 94.2(3) yes
C(25) Sn(3) C(26) 135.2(3) yes
Sn(1) O(10) Sn(2) 95.1(1) yes
Sn(1) O(10) C(2) 139.4(4) yes
Sn(2) O(10) C(2) 123.9(4) yes
Sn(3) O(19) N(18) 121.2(3) yes
Sn(1) O(20) C(12) 135.3(4) yes
Sn(1) O(30) Sn(2) 119.5(2) yes
Sn(1) O(30) Sn(3) 126.5(2) yes
Sn(2) O(30) Sn(3) 114.0(2) yes
Sn(2) O(40) Sn(3) 97.8(2) yes
Sn(2) O(40) N(4) 120.7(4) yes
Sn(3) O(40) N(4) 122.3(4) yes
O(40) N(4) C(41) 116.2(7) yes
Sn(1) N(8) O(9) 110.5(4) yes
Sn(1) N(8) C(7) 137.3(5) yes
O(9) N(8) C(7) 111.6(5) yes
Sn(1) N(18) O(19) 118.6(4) yes
Sn(1) N(18) C(17) 128.5(4) yes
O(19) N(18) C(17) 112.6(5) yes
C(2) C(1) C(6) 118.6(6) yes
C(2) C(1) C(7) 126.3(6) yes
C(6) C(1) C(7) 114.9(6) yes
O(10) C(2) C(1) 120.6(6) yes
O(10) C(2) C(3) 121.9(5) yes
C(1) C(2) C(3) 117.5(6) yes
C(2) C(3) C(4) 122.7(6) yes
C(3) C(4) C(5) 120.3(7) yes
C(4) C(5) C(6) 117.8(6) yes
C(1) C(6) C(5) 123.0(6) yes
N(8) C(7) C(1) 127.9(6) yes
C(12) C(11) C(16) 119.6(6) yes
C(12) C(11) C(17) 123.4(6) yes
C(16) C(11) C(17) 116.9(6) yes
O(20) C(12) C(11) 122.0(6) yes
O(20) C(12) C(13) 120.0(6) yes
C(11) C(12) C(13) 117.9(7) yes
C(12) C(13) C(14) 120.4(7) yes
C(13) C(14) C(15) 121.8(7) yes
C(14) C(15) C(16) 117.5(7) yes
C(11) C(16) C(15) 122.6(7) yes
N(18) C(17) C(11) 127.6(6) yes
N(4) C(41) C(42) 123.0(7) yes
C(41) C(42) C(43) 123.6(7) yes
C(41) C(42) C(47) 117.9(7) yes
C(43) C(42) C(47) 118.5(7) yes
C(42) C(43) C(44) 119.5(7) yes
C(43) C(44) C(45) 122.5(8) yes
C(44) C(45) C(46) 118.8(7) yes
C(45) C(46) C(47) 120.4(7) yes
C(42) C(47) C(46) 120.3(7) yes
C(102) C(101) C(103) 119(1) yes
C(101) C(102) C(103) 120(1) yes
C(101) C(103) C(102) 119(1) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn(1) O(10) 2.715(4) yes
Sn(1) O(20) 2.177(5) yes
Sn(1) O(30) 2.177(4) yes
Sn(1) N(8) 2.627(5) yes
Sn(1) N(18) 2.332(5) yes
Sn(1) C(21) 2.114(6) yes
Sn(1) C(22) 2.118(7) yes
Sn(2) O(10) 2.153(4) yes
Sn(2) O(30) 2.001(4) yes
Sn(2) O(40) 2.227(4) yes
Sn(2) C(23) 2.120(7) yes
Sn(2) C(24) 2.105(7) yes
Sn(3) O(19) 2.082(4) yes
Sn(3) O(30) 2.020(4) yes
Sn(3) O(40) 2.248(5) yes
Sn(3) C(25) 2.124(8) yes
Sn(3) C(26) 2.116(7) yes
O(9) N(8) 1.400(6) yes
O(10) C(2) 1.334(6) yes
O(19) N(18) 1.388(6) yes
O(20) C(12) 1.306(8) yes
O(40) N(4) 1.403(7) yes
N(4) C(41) 1.213(8) yes
N(8) C(7) 1.276(8) yes
N(18) C(17) 1.285(8) yes
C(1) C(2) 1.406(8) yes
C(1) C(6) 1.408(8) yes
C(1) C(7) 1.434(9) yes
C(2) C(3) 1.392(9) yes
C(3) C(4) 1.392(9) yes
C(4) C(5) 1.376(10) yes
C(5) C(6) 1.38(1) yes
C(11) C(12) 1.404(8) yes
C(11) C(16) 1.388(9) yes
C(11) C(17) 1.437(8) yes
C(12) C(13) 1.390(9) yes
C(13) C(14) 1.38(1) yes
C(14) C(15) 1.39(1) yes
C(15) C(16) 1.36(1) yes
C(41) C(42) 1.475(10) yes
C(42) C(43) 1.383(10) yes
C(42) C(47) 1.395(10) yes
C(43) C(44) 1.35(1) yes
C(44) C(45) 1.36(1) yes
C(45) C(46) 1.36(1) yes
C(46) C(47) 1.37(1) yes
C(101) C(102) 1.38(2) yes
C(101) C(103) 1.37(2) yes
C(102) C(103) 1.37(2) yes
