#------------------------------------------------------------------------------
#$Date: 2014-03-11 15:37:25 +0000 (Tue, 11 Mar 2014) $
#$Revision: 104835 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239003.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_2239003
loop_
_publ_author_name
'Gueye, Ndongo'
'Diop, Libasse'
'Stoeckli-Evans, Helen'
_publ_section_title
;
Tetrakis(dipropylammonium)
tetrakis(oxalato-\k^2^O^1^,O^2^)stannate(IV) monohydrate: a
complex with an eight-coordinate Sn^IV^ atom
;
_journal_coeditor_code WM2795
_journal_issue 2
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m49
_journal_page_last m50
_journal_paper_doi 10.1107/S160053681303496X
_journal_volume 70
_journal_year 2014
_chemical_formula_iupac '(C6 H16 N)4 [Sn (C2 O4)4] , H2 O'
_chemical_formula_moiety '4(C6 H16 N +), C8 O16 Sn 4-, H2 O'
_chemical_formula_sum 'C32 H66 N4 O17 Sn'
_chemical_formula_weight 897.57
_chemical_name_systematic
;
Tetrakis(dipropylammonium)
tetrakis(oxalato-\k^2^O^1^,O^2^)stannate(IV)
;
_space_group_crystal_system tetragonal
_space_group_IT_number 121
_space_group_name_Hall 'I -4 2'
_space_group_name_H-M_alt 'I -4 2 m'
_symmetry_space_group_name_Hall 'I -4 2'
_symmetry_space_group_name_H-M 'I -4 2 m'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary difmap
_atom_sites_solution_secondary geom
_audit_creation_method SHELXL-2013
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.5996(6)
_cell_length_b 14.5996(6)
_cell_length_c 9.5718(4)
_cell_measurement_reflns_used 16495
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 26.10
_cell_measurement_theta_min 1.97
_cell_volume 2040.21(15)
_computing_cell_refinement 'X-Area (Stoe & Cie, 2009)'
_computing_data_collection 'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction 'X-RED32 (Stoe & Cie, 2009)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and MERCURY (Macrae et al., 2006)'
_computing_publication_material
;
SHELXL-2013 (Sheldrick, 2008), PLATON (Spek, 2009) and
Publcif (Westrip, 2010)
;
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS2'
_diffrn_measurement_method '\f + \w scans'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0714
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 9636
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.628
_diffrn_reflns_theta_min 1.973
_exptl_absorpt_coefficient_mu 0.701
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.5398
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(MULscanABS in PLATON; Spek, 2009)'
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.461
_exptl_crystal_description rod
_exptl_crystal_F_000 944
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.22
_refine_diff_density_max 0.387
_refine_diff_density_min -0.618
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack 0.45(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.076
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 83
_refine_ls_number_reflns 1030
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0210
_refine_ls_R_factor_gt 0.0210
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.5457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0536
_refine_ls_wR_factor_ref 0.0537
_reflns_number_gt 1027
_reflns_number_total 1030
_reflns_threshold_expression 'I > 2\s(I)'
_[local]_cod_data_source_file wm2795sup1.cf
_[local]_cod_data_source_block I
_cod_original_cell_volume 2040.21(19)
_cod_database_code 2239003
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_checksum 4829
_shelx_hkl_file
;
12 13 -1 49.10 5.86
13 12 -1 58.91 5.85
12 12 -2 42.59 5.55
12 -12 2 30.30 4.19
12 -12 2 44.68 6.95
-12 -12 -2 35.12 5.88
12 12 -2 35.96 5.74
-12 -12 0 91.93 4.49
13 11 -2 51.44 3.98
13 -11 2 32.90 6.93
11 -13 2 35.75 6.84
11 13 -2 48.09 5.44
-11 -13 -2 38.44 4.45
13 11 -2 42.94 6.02
13 -11 2 35.19 5.96
11 -13 2 33.82 5.87
-13 -11 -2 33.96 4.16
11 13 -2 33.37 5.71
13 11 0 27.34 4.59
13 11 0 37.85 5.50
-11 -13 0 26.86 4.08
11 -12 3 18.76 6.13
12 11 -3 21.85 5.26
11 12 -3 31.69 5.18
12 11 -3 23.22 5.56
-12 -11 -3 26.14 5.77
11 -12 3 21.90 5.56
12 -11 3 29.90 5.65
12 -11 3 19.92 6.22
-11 -12 -3 34.60 5.88
11 -12 1 87.50 5.78
-12 -11 -1 99.55 5.56
11 12 -1 81.84 5.87
12 -11 1 78.06 6.81
12 -11 1 102.80 5.87
12 11 -1 124.28 5.45
11 12 -1 118.87 5.51
11 -12 1 95.85 7.07
12 11 -1 99.04 6.22
-11 -12 -1 94.64 5.76
11 -11 4 78.31 4.47
11 -11 4 58.17 4.64
11 11 -4 111.17 5.63
-11 -11 -4 94.09 6.36
11 -11 2 91.77 6.62
11 -11 2 102.93 5.76
11 11 -2 108.60 3.97
11 11 -2 83.58 5.64
-11 -11 -2 89.00 5.71
-11 -11 0 79.41 5.22
10 14 -2 40.69 4.11
10 -14 2 27.62 5.19
-10 -14 -2 39.43 6.20
14 -10 2 30.38 4.42
14 10 -2 42.67 7.89
14 -10 2 35.77 6.96
-14 -10 -2 38.96 5.86
10 -14 2 33.94 6.16
14 10 -2 36.03 5.77
14 10 0 32.02 4.14
-10 -14 0 34.45 5.73
14 10 0 40.72 6.67
10 -13 3 26.54 4.04
13 -10 3 29.44 6.32
13 10 -3 28.88 4.07
13 10 -3 29.85 7.26
-10 -13 -3 25.26 4.49
10 -13 3 20.58 6.65
-13 -10 -3 29.89 5.85
10 13 -3 32.32 5.16
13 -10 3 27.08 5.79
13 10 -1 32.42 6.23
10 -13 1 22.43 4.92
10 -13 1 24.81 5.75
-10 -13 -1 22.12 4.17
13 -10 1 34.33 5.69
13 -10 1 22.11 4.72
-13 -10 -1 37.06 5.32
10 13 -1 28.87 5.30
10 13 -1 29.74 3.87
13 10 -1 36.48 5.19
10 -12 4 32.60 4.56
10 12 -4 45.27 5.43
10 -12 4 37.51 4.20
-12 -10 -4 41.65 4.31
12 10 -4 42.24 3.86
12 10 -4 30.73 7.00
-10 -12 -4 35.35 5.90
12 -10 4 30.31 4.17
12 -10 4 42.41 6.10
10 12 -2 91.02 5.63
10 -12 2 89.03 6.71
12 -10 2 89.73 4.37
12 10 -2 95.92 5.95
12 -10 2 86.96 4.89
-10 -12 -2 93.12 4.28
-12 -10 -2 97.89 5.55
10 12 -2 116.16 5.23
12 10 -2 108.89 4.05
10 -12 2 99.92 5.66
-10 -12 0 22.42 4.99
12 10 0 28.72 4.94
12 10 0 21.90 5.95
11 -10 5 44.41 4.25
10 -11 5 44.99 4.40
-11 -10 -5 66.85 5.99
-10 -11 -5 53.51 6.21
10 -11 5 62.73 5.78
11 10 -5 68.67 5.50
10 11 -5 76.60 5.49
11 -10 5 50.92 4.31
10 11 -3 109.01 5.74
-11 -10 -3 112.09 4.39
11 -10 3 117.22 4.42
11 -10 3 97.09 4.69
10 -11 3 129.88 6.36
-10 -11 -3 122.86 4.59
11 10 -3 142.00 4.12
10 -11 3 132.23 5.82
10 11 -3 155.63 5.34
11 10 -3 133.64 6.76
10 -11 1 233.53 6.38
10 11 -1 229.51 4.52
11 10 -1 259.85 5.70
10 -11 1 213.37 7.07
11 -10 1 186.29 5.03
10 11 -1 202.91 6.04
11 10 -1 213.64 6.50
-11 -10 -1 211.27 5.96
11 -10 1 207.38 6.96
-10 -11 -1 224.99 6.04
10 -10 6 118.18 4.69
-10 -10 -6 116.95 6.79
10 10 -6 127.67 4.42
10 -10 6 95.47 6.04
10 10 -4 148.83 4.28
10 -10 4 112.85 6.08
10 -10 4 124.11 4.44
-10 -10 -4 132.02 4.49
10 10 -2 143.90 5.72
10 -10 2 154.54 4.55
10 10 -2 192.13 5.22
-10 -10 -2 174.79 5.77
10 -10 2 140.24 4.72
-10 -10 0 572.50 7.69
15 9 -2 43.67 6.00
9 15 -2 36.36 4.18
15 9 0 35.36 5.77
-9 -15 0 25.28 5.96
15 9 0 33.22 6.95
9 14 -3 74.21 5.44
9 -14 3 40.12 5.02
14 9 -3 63.14 5.83
14 9 -3 61.66 8.00
14 -9 3 56.18 6.80
-14 -9 -3 55.82 4.33
14 -9 3 51.12 4.59
-9 -14 -3 60.18 6.55
9 -14 3 52.66 6.09
14 9 -1 38.59 3.91
14 -9 1 37.72 4.46
14 9 -1 41.77 6.56
-9 -14 -1 35.57 5.64
9 -14 1 51.23 6.11
14 -9 1 43.39 6.53
9 14 -1 36.34 5.39
-14 -9 -1 36.04 5.68
9 -14 1 27.39 5.10
9 13 -4 33.94 5.03
13 -9 4 21.07 6.09
9 -13 4 33.34 5.80
9 -13 4 26.65 6.30
13 -9 4 30.52 5.80
-13 -9 -4 31.80 5.85
13 9 -4 25.98 5.50
13 9 -4 20.46 7.02
-9 -13 -4 31.19 4.48
9 13 -2 73.71 3.86
13 9 -2 63.51 6.26
13 9 -2 74.69 5.38
9 -13 2 65.53 4.21
-9 -13 -2 65.99 5.77
-13 -9 -2 61.26 5.49
13 -9 2 78.91 6.48
9 -13 2 59.04 6.62
13 -9 2 66.15 5.91
-9 -13 0 28.82 3.84
13 9 0 38.28 5.05
13 9 0 34.23 6.34
-9 -12 -5 50.50 6.38
9 -12 5 26.00 6.19
12 -9 5 32.48 5.92
9 -12 5 32.17 5.90
9 12 -5 39.39 5.14
12 9 -5 31.17 5.32
12 -9 5 32.95 4.20
-12 -9 -5 23.33 4.37
-12 -9 -3 122.02 5.92
9 -12 3 122.36 6.59
12 -9 3 128.30 4.70
12 9 -3 113.23 6.18
9 -12 3 138.95 6.02
-9 -12 -3 130.14 6.07
12 9 -3 159.43 5.68
9 12 -3 149.64 5.30
12 -9 3 126.90 6.45
-9 -12 -1 82.50 5.22
9 12 -1 87.09 3.69
12 9 -1 90.09 5.05
9 12 -1 80.88 5.07
12 9 -1 83.39 6.11
12 -9 1 83.28 4.19
9 -12 1 76.70 6.71
-12 -9 -1 75.05 3.84
12 -9 1 79.38 4.62
9 -12 1 66.57 4.13
9 11 -6 84.84 5.72
9 -11 6 60.77 4.61
9 -11 6 48.16 4.31
-9 -11 -6 68.05 6.55
11 -9 6 63.94 5.88
11 -9 6 77.21 5.93
-11 -9 -6 71.97 6.27
11 9 -6 77.61 5.67
11 9 -4 73.48 7.63
9 -11 4 63.03 4.36
9 -11 4 93.26 5.61
-9 -11 -4 88.36 5.81
-11 -9 -4 85.52 5.61
11 -9 4 83.57 5.79
11 9 -4 87.98 3.91
11 -9 4 76.22 5.91
9 11 -4 88.72 3.85
9 11 -2 137.01 5.75
11 9 -2 136.56 6.14
9 -11 2 161.06 5.61
11 -9 2 130.31 4.71
11 -9 2 139.93 4.48
11 9 -2 168.94 5.15
-9 -11 -2 149.61 4.36
9 -11 2 132.53 6.26
9 11 -2 161.50 5.08
-11 -9 -2 149.53 5.46
11 9 0 253.88 6.89
-9 -11 0 224.35 4.63
11 9 0 261.33 5.63
10 9 -7 49.56 5.72
9 -10 7 31.22 4.37
9 10 -7 44.18 5.56
10 -9 7 29.66 5.79
-9 -10 -7 40.57 6.79
10 -9 7 41.31 4.37
-10 -9 -7 43.51 6.69
9 -10 7 41.86 6.14
9 -10 5 126.74 5.93
-9 -10 -5 141.48 6.17
10 9 -5 166.12 5.56
9 -10 5 141.79 4.48
-10 -9 -5 154.35 6.05
10 -9 5 130.08 5.77
10 -9 5 142.03 4.63
9 10 -5 172.69 5.50
10 -9 3 146.59 6.03
-9 -10 -3 150.21 4.37
9 -10 3 141.77 4.38
-10 -9 -3 141.32 4.18
9 10 -3 179.76 5.08
10 9 -3 166.46 4.20
9 -10 3 141.68 6.05
9 10 -3 141.46 5.70
10 -9 3 148.75 4.30
10 9 -3 139.75 6.71
9 10 -1 236.62 5.32
10 9 -1 213.69 6.28
9 -10 1 203.63 6.63
9 10 -1 199.02 5.86
-10 -9 -1 199.15 4.25
10 9 -1 238.09 5.29
-9 -10 -1 205.61 5.64
10 -9 1 211.61 6.55
10 -9 1 223.39 5.99
9 -10 1 189.63 4.61
9 -9 8 78.76 4.81
-9 -9 -8 73.32 7.70
9 -9 8 49.83 6.55
9 9 -8 81.32 6.31
9 9 -6 58.65 5.28
9 -9 6 48.44 5.42
-9 -9 -6 55.33 5.87
9 -9 6 49.39 5.52
9 -9 4 90.56 4.25
9 -9 4 134.95 4.18
9 9 -4 155.75 5.28
-9 -9 -4 118.26 4.22
-9 -9 -2 108.82 3.78
9 9 -2 133.37 4.62
9 9 -2 98.24 5.08
9 -9 2 108.34 5.71
9 -9 2 97.83 3.91
-9 -9 0 502.36 6.65
8 15 -3 38.83 4.07
8 -15 3 27.66 5.14
15 -8 3 34.52 6.77
15 8 -3 37.82 5.86
8 -15 3 32.45 4.54
15 -8 3 34.72 4.70
-8 -15 -3 39.53 6.72
-8 -15 -3 43.87 6.72
15 8 -3 34.90 6.87
-15 -8 -3 27.52 4.38
15 8 -1 44.64 6.79
-8 -15 -1 44.82 6.05
8 15 -1 60.46 5.44
8 -15 1 48.72 7.33
15 8 -1 48.33 4.17
-15 -8 -1 43.75 5.74
8 -15 1 34.31 4.75
-8 -15 -1 37.00 4.95
15 -8 1 37.76 6.90
14 -8 4 35.89 6.31
-8 -14 -4 35.87 4.89
8 14 -4 44.55 5.19
14 -8 4 41.34 4.52
8 -14 4 34.60 5.94
14 8 -4 52.15 5.86
14 8 -4 36.07 7.94
8 -14 4 31.29 6.54
-14 -8 -4 32.02 4.37
-8 -14 -2 86.99 6.64
8 14 -2 93.34 5.38
-14 -8 -2 58.69 4.25
8 -14 2 69.55 4.39
14 8 -2 83.80 6.78
14 -8 2 69.07 4.81
8 -14 2 70.37 6.93
14 -8 2 80.07 4.58
14 8 -2 93.02 4.14
-8 -14 -2 75.49 4.50
14 8 0 52.77 6.75
14 8 0 47.27 5.22
-8 -14 0 42.29 5.45
-8 -14 0 33.56 4.73
8 -13 5 42.00 4.55
13 -8 5 56.27 5.97
8 -13 5 56.27 4.50
13 8 -5 59.58 4.06
13 -8 5 65.78 5.86
-8 -13 -5 62.30 6.45
-13 -8 -5 52.65 6.18
8 13 -5 50.79 5.41
13 8 -3 150.48 8.00
13 -8 3 131.03 4.84
-13 -8 -3 129.00 5.84
13 -8 3 123.84 6.59
-8 -13 -3 120.68 4.96
13 8 -3 152.26 5.71
8 -13 3 134.88 5.93
8 -13 3 123.58 6.49
-8 -13 -3 132.97 6.44
8 13 -3 123.00 4.00
8 13 -1 111.93 3.86
8 -13 1 133.21 6.04
8 13 -1 118.61 5.52
-8 -13 -1 94.30 4.92
13 8 -1 131.50 6.67
-8 -13 -1 110.85 5.59
13 8 -1 131.76 5.39
13 -8 1 93.79 4.89
8 -13 1 98.63 5.12
-13 -8 -1 124.48 5.42
8 -12 6 27.75 6.21
12 -8 6 38.96 5.60
12 8 -6 41.54 4.14
-12 -8 -6 41.59 6.20
12 -8 6 35.15 4.12
-8 -12 -6 40.42 6.60
8 -12 6 33.32 4.25
8 12 -6 39.21 5.17
8 -12 4 117.18 4.48
-8 -12 -4 127.82 6.43
8 -12 4 112.33 6.19
12 -8 4 152.80 6.08
-12 -8 -4 140.17 5.96
12 8 -4 120.14 7.66
8 12 -4 139.61 5.30
12 -8 4 115.91 4.72
12 8 -4 136.42 4.32
-8 -12 -2 193.26 4.77
8 -12 2 182.13 6.45
8 12 -2 232.94 5.39
12 -8 2 242.36 6.57
8 -12 2 202.75 5.93
12 8 -2 174.42 6.65
12 -8 2 197.13 6.79
12 8 -2 222.34 4.58
-12 -8 -2 190.62 4.62
12 8 0 72.49 4.88
-8 -12 0 63.85 3.79
12 8 0 74.64 6.06
11 -8 7 39.57 6.08
-8 -11 -7 41.53 7.02
11 8 -7 46.63 4.35
11 -8 7 38.50 6.05
8 -11 7 43.33 6.29
8 11 -7 51.85 5.50
8 -11 7 27.97 6.11
-11 -8 -7 49.38 6.51
8 -11 5 90.53 5.68
11 -8 5 87.05 4.25
8 11 -5 104.92 5.22
-11 -8 -5 91.19 5.74
11 -8 5 68.99 4.21
8 -11 5 93.06 5.85
-8 -11 -5 75.69 4.54
11 8 -5 95.64 5.41
-11 -8 -3 90.64 5.12
8 -11 3 87.31 4.00
11 8 -3 96.71 5.02
8 11 -3 89.13 4.72
8 -11 3 69.77 4.31
-8 -11 -3 101.90 5.50
11 -8 3 84.07 4.22
11 -8 3 85.90 5.73
11 8 -3 79.53 5.88
8 11 -1 139.41 3.75
11 -8 1 168.38 5.88
8 -11 1 149.61 5.48
11 8 -1 157.85 3.89
11 -8 1 147.81 6.25
8 11 -1 139.28 5.22
-11 -8 -1 137.16 3.91
11 8 -1 158.87 6.24
8 -11 1 118.42 4.70
-8 -11 -1 141.43 4.12
10 -8 8 29.02 6.15
10 -8 8 20.06 6.31
8 10 -8 36.11 5.87
-10 -8 -8 35.21 7.34
8 -10 8 18.52 4.70
8 -10 8 34.07 6.23
10 8 -8 29.11 6.22
-8 -10 -6 38.35 5.91
10 -8 6 33.43 5.28
8 10 -6 37.71 3.65
8 -10 6 40.81 5.28
10 8 -6 42.78 5.21
-10 -8 -6 37.30 5.80
8 -10 6 34.72 3.88
10 -8 6 40.59 5.42
-10 -8 -4 75.61 3.77
10 8 -4 65.57 6.61
-8 -10 -4 83.64 5.45
8 -10 4 77.10 5.42
10 -8 4 88.04 5.59
8 10 -4 83.23 3.44
10 8 -4 89.87 3.67
10 -8 4 77.16 5.65
8 -10 4 82.01 3.98
10 -8 2 48.11 4.89
8 10 -2 48.97 4.26
10 -8 2 34.75 3.84
8 -10 2 35.87 4.76
8 10 -2 38.61 5.46
10 8 -2 43.86 5.04
10 8 -2 48.59 4.27
8 -10 2 38.71 3.74
-10 -8 -2 35.99 3.32
-8 -10 -2 48.02 4.58
-8 -10 0 137.72 4.82
10 8 0 143.94 6.01
10 8 0 140.46 3.77
-8 -9 -7 33.62 4.60
9 8 -7 45.25 4.01
-9 -8 -7 34.55 6.28
8 9 -7 48.53 5.27
8 -9 7 28.08 5.71
9 -8 7 32.90 4.05
8 -9 7 39.12 5.75
9 -8 7 33.98 4.11
9 -8 5 125.71 5.50
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;
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TITL NDG470 IPDS2 -100DEGC I-42M
CELL 0.71073 14.59960 14.59960 9.57180 90.00000 90.00000 90.00000
ZERR 2 0.00060 0.00060 0.00040 0.00000 0.00000 0.00000
LATT -2
SYMM X, -Y, -Z
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM -Y, -X, Z
SYMM -Y, X, -Z
SYMM Y, -X, -Z
SYMM Y, X, Z
SFAC C H N O SN
UNIT 64 132 8 34 2
TEMP -100
L.S. 11
FMAP 2
PLAN 20
ACTA
BOND $H
DFIX 0.84 .02 O1W H1WA
DFIX 0.88 .02 N1 H1AN N1 H1BN
HTAB
EQIV $1 -X+1/2, -Y+1/2, Z-1/2
HTAB N1 O1_$1
HTAB N1 O2_$1
HTAB N1 O2
HTAB N1 O4
EQIV $2 X-1/2, Y-1/2, Z+1/2
HTAB O1W O3_$2
CONF
TWIN
WGHT 0.030000 1.545700
BASF 0.45217
FVAR 0.28615
SN1 5 0.500000 0.500000 0.500000 10.12500 0.02109 0.02109 =
0.01231 0.00000 0.00000 0.00000
O1 4 0.401109 0.401109 0.567539 10.50000 0.03518 0.03518 =
0.01897 -0.00197 -0.00197 -0.01174
O2 4 0.297432 0.297432 0.507869 10.50000 0.04173 0.04173 =
0.02340 -0.00015 -0.00015 -0.01875
O3 4 0.438910 0.438910 0.308425 10.50000 0.03464 0.03464 =
0.01514 -0.00256 -0.00256 -0.00885
O4 4 0.336638 0.336638 0.230471 10.50000 0.05478 0.05478 =
0.02110 -0.00443 -0.00443 -0.02577
C1 1 0.355864 0.355864 0.477784 10.50000 0.02984 0.02984 =
0.02319 -0.00203 -0.00203 -0.00101
C2 1 0.377591 0.377591 0.323091 10.50000 0.02726 0.02726 =
0.02015 -0.00062 -0.00062 -0.00320
N1 3 0.192119 0.192119 0.320172 10.50000 0.03230 0.03230 =
0.02222 -0.00294 -0.00294 -0.00826
H1AN 2 0.194549 0.194549 0.228486 10.50000 -1.20000
H1BN 2 0.232234 0.232234 0.350448 10.50000 -1.20000
C3 1 0.098460 0.217410 0.368648 11.00000 0.03556 0.04894 =
0.02620 0.00145 0.00257 0.00090
AFIX 23
H3A 2 0.094670 0.208702 0.471057 11.00000 -1.20000
H3B 2 0.053235 0.175985 0.324523 11.00000 -1.20000
AFIX 0
C4 1 0.074111 0.315883 0.333515 11.00000 0.05607 0.05362 =
0.03272 -0.00456 -0.00081 0.01482
AFIX 23
H4A 2 0.015959 0.331501 0.381085 11.00000 -1.20000
H4B 2 0.122289 0.356396 0.371974 11.00000 -1.20000
AFIX 0
C5 1 0.063715 0.336143 0.180058 11.00000 0.06389 0.05053 =
0.03478 0.00539 -0.00002 0.00202
AFIX 137
H5A 2 0.123203 0.329610 0.133685 11.00000 -1.50000
H5B 2 0.041278 0.398901 0.167879 11.00000 -1.50000
H5C 2 0.019900 0.293100 0.138752 11.00000 -1.50000
AFIX 0
O1W 4 0.000000 -0.026444 0.500000 10.12500 0.14985 0.06540 =
0.05709 0.00000 0.01067 0.00000
AFIX 3
H1WA 2 -0.016700 -0.035472 0.584000 10.25000 -1.50000
AFIX 0
HKLF 4
REM NDG470 IPDS2 -100DEGC I-42M
REM R1 = 0.0210 for 1027 Fo > 4sig(Fo) and 0.0210 for all 1030 data
REM 83 parameters refined using 3 restraints
END
WGHT 0.0303 1.6751
REM Instructions for potential hydrogen bonds
HTAB N1 O1_$1
HTAB N1 O2_$1
HTAB N1 O2
HTAB N1 O4
HTAB O1W O3_$2
REM Highest difference peak 0.387, deepest hole -0.618, 1-sigma level 0.050
Q1 1 0.4448 0.4448 0.4996 10.50000 0.05 0.39
Q2 1 0.5089 0.4252 0.3919 11.00000 0.05 0.22
Q3 1 0.4490 0.4490 0.3718 10.50000 0.05 0.18
Q4 1 0.5033 0.3864 0.3185 11.00000 0.05 0.18
Q5 1 0.0000 0.2895 0.5000 10.50000 0.05 0.15
Q6 1 0.4430 0.4650 0.6249 11.00000 0.05 0.15
Q7 1 0.0003 0.3902 0.1522 11.00000 0.05 0.14
Q8 1 -0.0355 0.2769 0.2694 11.00000 0.05 0.14
Q9 1 0.3968 0.5280 0.3262 11.00000 0.05 0.14
Q10 1 0.5000 0.5993 0.5000 10.50000 0.05 0.13
Q11 1 0.4716 0.3490 0.5829 11.00000 0.05 0.13
Q12 1 0.4007 0.4982 0.5715 11.00000 0.05 0.12
Q13 1 0.5000 0.5000 0.3232 10.25000 0.05 0.12
Q14 1 -0.0037 0.2971 0.3496 11.00000 0.05 0.12
Q15 1 0.3535 0.3329 0.4937 11.00000 0.05 0.11
Q16 1 0.4549 0.3554 0.4177 11.00000 0.05 0.11
Q17 1 0.2837 0.3385 0.5006 11.00000 0.05 0.11
Q18 1 0.0760 0.1191 0.3576 11.00000 0.05 0.11
Q19 1 0.1357 0.3975 0.2219 11.00000 0.05 0.11
Q20 1 0.3586 0.3586 0.5886 10.50000 0.05 0.11
;
_shelxl_version_number 2.013
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, -z'
'-x, -y, z'
'-x, y, -z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Sn Sn1 0.5000 0.5000 0.5000 0.01816(16) Uani d 1
O O1 0.40111(16) 0.40111(16) 0.5675(4) 0.0298(8) Uani d 1
O O2 0.29743(14) 0.29743(14) 0.5079(8) 0.0356(7) Uani d 1
O O3 0.43891(16) 0.43891(16) 0.3084(3) 0.0281(7) Uani d 1
O O4 0.3366(2) 0.3366(2) 0.2305(4) 0.0436(10) Uani d 1
C C1 0.3559(2) 0.3559(2) 0.4778(6) 0.0276(13) Uani d 1
C C2 0.3776(2) 0.3776(2) 0.3231(5) 0.0249(9) Uani d 1
N N1 0.1921(2) 0.1921(2) 0.3202(5) 0.0289(9) Uani d 1
H H1AN 0.195(3) 0.195(3) 0.228(3) 0.035 Uiso d 1
H H1BN 0.2322(15) 0.2322(15) 0.350(6) 0.035 Uiso d 1
C C3 0.0985(3) 0.2174(3) 0.3686(4) 0.0369(8) Uani d 1
H H3A 0.0947 0.2087 0.4711 0.044 Uiso calc 1
H H3B 0.0532 0.1760 0.3245 0.044 Uiso calc 1
C C4 0.0741(3) 0.3159(3) 0.3335(4) 0.0475(10) Uani d 1
H H4A 0.0160 0.3315 0.3811 0.057 Uiso calc 1
H H4B 0.1223 0.3564 0.3720 0.057 Uiso calc 1
C C5 0.0637(3) 0.3361(3) 0.1801(4) 0.0497(10) Uani d 1
H H5A 0.1232 0.3296 0.1337 0.075 Uiso calc 1
H H5B 0.0413 0.3989 0.1679 0.075 Uiso calc 1
H H5C 0.0199 0.2931 0.1388 0.075 Uiso calc 1
O O1W 0.0000 -0.026(3) 0.5000 0.091(15) Uani d 0.25
H H1WA -0.0167 -0.0355 0.5840 0.136 Uiso d 0.25
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn1 0.02109(19) 0.02109(19) 0.0123(2) 0.000 0.000 0.000
O1 0.0352(12) 0.0352(12) 0.0190(15) -0.0117(16) -0.0020(10) -0.0020(10)
O2 0.0417(10) 0.0417(10) 0.0234(17) -0.0187(13) -0.0001(18) -0.0001(18)
O3 0.0346(11) 0.0346(11) 0.0151(14) -0.0089(14) -0.0026(9) -0.0026(9)
O4 0.0548(17) 0.0548(17) 0.0211(19) -0.026(2) -0.0044(12) -0.0044(12)
C1 0.0298(13) 0.0298(13) 0.023(4) -0.0010(17) -0.0020(15) -0.0020(15)
C2 0.0273(14) 0.0273(14) 0.020(2) -0.0032(18) -0.0006(13) -0.0006(13)
N1 0.0323(14) 0.0323(14) 0.022(2) -0.0083(18) -0.0029(13) -0.0029(13)
C3 0.0356(19) 0.049(2) 0.0262(17) 0.0009(16) 0.0026(14) 0.0014(16)
C4 0.056(3) 0.054(3) 0.033(2) 0.015(2) -0.0008(19) -0.0046(18)
C5 0.064(3) 0.051(3) 0.035(2) 0.002(2) 0.000(2) 0.0054(18)
O1W 0.15(5) 0.065(15) 0.057(7) 0.000 0.01(3) 0.000
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Sn1 O1 3_665 4_656 95.23(5)
O1 Sn1 O1 3_665 2_566 95.23(5)
O1 Sn1 O1 4_656 2_566 144.86(18)
O1 Sn1 O1 3_665 . 144.86(18)
O1 Sn1 O1 4_656 . 95.23(5)
O1 Sn1 O1 2_566 . 95.23(5)
O1 Sn1 O3 3_665 . 142.09(12)
O1 Sn1 O3 4_656 . 75.60(8)
O1 Sn1 O3 2_566 . 75.60(8)
O1 Sn1 O3 . . 73.05(13)
O1 Sn1 O3 3_665 4_656 75.60(8)
O1 Sn1 O3 4_656 4_656 73.05(13)
O1 Sn1 O3 2_566 4_656 142.09(12)
O1 Sn1 O3 . 4_656 75.60(8)
O3 Sn1 O3 . 4_656 132.75(11)
O1 Sn1 O3 3_665 2_566 75.60(8)
O1 Sn1 O3 4_656 2_566 142.09(12)
O1 Sn1 O3 2_566 2_566 73.05(13)
O1 Sn1 O3 . 2_566 75.60(8)
O3 Sn1 O3 . 2_566 132.75(11)
O3 Sn1 O3 4_656 2_566 69.05(17)
O1 Sn1 O3 3_665 3_665 73.05(13)
O1 Sn1 O3 4_656 3_665 75.60(8)
O1 Sn1 O3 2_566 3_665 75.60(8)
O1 Sn1 O3 . 3_665 142.09(12)
O3 Sn1 O3 . 3_665 69.05(17)
O3 Sn1 O3 4_656 3_665 132.75(11)
O3 Sn1 O3 2_566 3_665 132.75(11)
C1 O1 Sn1 . . 119.8(3)
C2 O3 Sn1 . . 118.2(3)
O2 C1 O1 . . 124.0(6)
O2 C1 C2 . . 120.3(5)
O1 C1 C2 . . 115.7(4)
O4 C2 O3 . . 127.3(4)
O4 C2 C1 . . 119.5(4)
O3 C2 C1 . . 113.2(4)
C3 N1 C3 . 8 111.0(4)
C3 N1 H1AN . . 110(2)
C3 N1 H1AN 8 . 110(2)
C3 N1 H1BN . . 110.1(19)
C3 N1 H1BN 8 . 110.1(19)
H1AN N1 H1BN . . 106(6)
N1 C3 C4 . . 112.4(3)
N1 C3 H3A . . 109.1
C4 C3 H3A . . 109.1
N1 C3 H3B . . 109.1
C4 C3 H3B . . 109.1
H3A C3 H3B . . 107.9
C5 C4 C3 . . 115.2(4)
C5 C4 H4A . . 108.5
C3 C4 H4A . . 108.5
C5 C4 H4B . . 108.5
C3 C4 H4B . . 108.5
H4A C4 H4B . . 107.5
C4 C5 H5A . . 109.5
C4 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C4 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
O1W O1W O1W 5 7_556 90.004(7)
O1W O1W O1W 5 2_556 45.002(4)
O1W O1W O1W 7_556 2_556 45.002(4)
O1W O1W H1WA 5 . 108.2
O1W O1W H1WA 7_556 . 84.7
O1W O1W H1WA 2_556 . 98.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn1 O1 3_665 2.142(3)
Sn1 O1 4_656 2.142(3)
Sn1 O1 2_566 2.142(3)
Sn1 O1 . 2.142(3)
Sn1 O3 . 2.226(3)
Sn1 O3 4_656 2.226(3)
Sn1 O3 2_566 2.226(3)
Sn1 O3 3_665 2.226(3)
O1 C1 . 1.269(6)
O2 C1 . 1.240(6)
O3 C2 . 1.274(6)
O4 C2 . 1.225(6)
C1 C2 . 1.547(7)
N1 C3 . 1.490(4)
N1 C3 8 1.490(4)
N1 H1AN . 0.88(3)
N1 H1BN . 0.88(3)
C3 C4 . 1.519(6)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 C5 . 1.506(5)
C4 H4A . 0.9900
C4 H4B . 0.9900
C5 H5A . 0.9800
C5 H5B . 0.9800
C5 H5C . 0.9800
O1W O1W 5 0.55(6)
O1W O1W 7_556 0.55(6)
O1W O1W 2_556 0.77(8)
O1W H1WA . 0.8505
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1AN O1 11_554 0.88(3) 2.50(5) 3.091(6) 125(5)
N1 H1AN O2 11_554 0.88(3) 2.12(3) 2.997(8) 179(6)
N1 H1BN O2 . 0.88(3) 2.02(4) 2.821(7) 151(5)
N1 H1BN O4 . 0.88(3) 2.44(5) 3.105(6) 133(5)
O1W H1WA O3 9_445 0.85 2.27 3.125(7) 179
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_site_symmetry_1
_geom_torsion
Sn1 O1 C1 O2 . 180.000000
Sn1 O1 C1 C2 . 0.0000(10)
Sn1 O3 C2 O4 . 180.000000
Sn1 O3 C2 C1 . 0.0000(10)
O2 C1 C2 O4 . 0.0000(10)
O1 C1 C2 O4 . 180.0000(10)
O2 C1 C2 O3 . 180.000000
O1 C1 C2 O3 . 0.0000(10)
C3 N1 C3 C4 8 174.3(3)
N1 C3 C4 C5 . 67.2(5)
_cod_database_fobs_code 2239003