#------------------------------------------------------------------------------
#$Date: 2013-12-09 14:40:51 +0000 (Mon, 09 Dec 2013) $
#$Revision: 91231 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238812.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238812
loop_
_publ_author_name
'Sarr, Modou'
'Diallo, Waly'
'Diasse-Sarr, Aminata'
'Plasseraud, Laurent'
'Cattey, H\'el\`ene'
_publ_section_title
;
Tris(cyclohexylammonium)
cis-dichloridobis(oxalato-\k^2^O^1^,O^2^)stannate(IV)
chloride monohydrate
;
_journal_coeditor_code WM2771
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m581
_journal_page_last m582
_journal_paper_doi 10.1107/S1600536813026901
_journal_volume 69
_journal_year 2013
_chemical_formula_iupac '(C6 H14 N)3 [Sn (C2 O4)2 Cl2] Cl, H2 O'
_chemical_formula_moiety '3(C6 H14 N +), C4 Cl2 O8 Sn 2-, Cl -, H2 O'
_chemical_formula_sum 'C22 H44 Cl3 N3 O9 Sn'
_chemical_formula_weight 719.64
_chemical_name_systematic
;
Tris(cyclohexylammonium)
cis-dichloridobis(oxalato-\k^2^O^1^,O^2^)stannate(IV)
chloride monohydrate
;
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/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 105.5420(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 27.9894(10)
_cell_length_b 12.3088(5)
_cell_length_c 19.3457(7)
_cell_measurement_reflns_used 59056
_cell_measurement_temperature 115(2)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 0.998
_cell_volume 6421.2(4)
_computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection 'COLLECT (Nonius, 1998)'
_computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 2012) and Mercury (Macrae et al., 2008)'
_computing_publication_material 'WinGX (Farrugia, 2012)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature 115(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans (\k = 0) + additional \w scans'
_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 0.0283
_diffrn_reflns_av_sigmaI/netI 0.0379
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 10624
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 2.97
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.093
_exptl_absorpt_correction_type none
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.489
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 2960
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.658
_refine_diff_density_min -0.696
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.223
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 346
_refine_ls_number_reflns 7264
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.223
_refine_ls_R_factor_all 0.0674
_refine_ls_R_factor_gt 0.0490
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+39.7649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0865
_refine_ls_wR_factor_ref 0.0947
_reflns_number_gt 6028
_reflns_number_total 7264
_reflns_threshold_expression I>2sigma(I)
_[local]_cod_data_source_file wm2771.cif
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'C 2/c'
_cod_database_code 2238812
_shelx_hkl_checksum 31586
_shelx_hkl_file
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;
TITL 1210b10
CELL 0.71073 27.9894 12.3088 19.3457 90.000 105.542 90.000
ZERR 8.00 0.0010 0.0005 0.0007 0.000 0.001 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H CL N O SN
UNIT 176 352 24 24 72 8
MERG 2
OMIT 2 0 0
OMIT 1 1 0
OMIT -1 1 2
OMIT 0 0 2
OMIT -1 1 1
OMIT -4 0 6
OMIT 1 1 1
OMIT -3 1 4
OMIT -7 1 2
OMIT -6 0 22
OMIT 1 3 1
OMIT 5 1 0
OMIT 4 2 3
OMIT -2 2 1
OMIT 8 0 22
OMIT 19 11 8
OMIT 2 14 0
EQIV $1 x, y+1, z
EQIV $2 -x+3/2, y+1/2, -z+1/2
EQIV $3 -x+3/2, -y+1/2, -z
EQIV $4 x, -y, z+1/2
HTAB N1 O4_$2
HTAB N1 CL3_$2
HTAB N1 O8
HTAB N1 O7
HTAB N2 O4_$1
HTAB N2 O3_$1
HTAB N2 CL3_$2
HTAB N2 O6_$3
HTAB N3 CL3
HTAB N3 O7
HTAB N3 O9
HTAB N3 O1_$4
HTAB O9 CL3_$2
HTAB O9 O3_$4
MPLA 4 O1 C1 C2 O2
MPLA 4 O5 C3 C4 O6
FMAP 2
PLAN 5
SIZE 0.030 0.080 0.170
ACTA
BOND $H
L.S. 5
TEMP 20.00
WGHT 0.000000 39.764904
FVAR 0.13977
MOLE 1
SN 6 0.844813 -0.012638 0.086704 11.00000 0.02068 0.02730 =
0.01990 0.00308 0.00525 -0.00111
O1 5 0.821369 -0.134292 0.009135 11.00000 0.03419 0.02951 =
0.02055 0.00074 0.01032 -0.00045
O2 5 0.816933 -0.130359 0.143988 11.00000 0.02854 0.02537 =
0.02118 0.00016 0.00857 -0.00178
O3 5 0.798993 -0.309233 -0.001369 11.00000 0.03871 0.03033 =
0.02576 -0.00384 0.01019 0.00311
O4 5 0.795341 -0.304088 0.140460 11.00000 0.04208 0.02794 =
0.02409 0.00188 0.01243 -0.00282
O5 5 0.848183 0.097220 0.168215 11.00000 0.02986 0.02763 =
0.02594 0.00157 0.00819 0.00216
O6 5 0.771567 0.044529 0.057607 11.00000 0.02527 0.02978 =
0.02280 -0.00392 -0.00070 0.00250
O8 5 0.723531 0.168183 0.089016 11.00000 0.03142 0.04578 =
0.03226 -0.00293 0.00800 0.01018
O7 5 0.801294 0.217365 0.206947 11.00000 0.04560 0.03048 =
0.02392 -0.00571 0.01015 -0.00469
CL1 3 0.925079 -0.080248 0.132803 11.00000 0.02245 0.05385 =
0.04968 0.01406 0.01075 0.00532
CL2 3 0.862379 0.105937 0.001742 11.00000 0.05407 0.04393 =
0.03392 0.01339 0.01745 -0.00588
C3 1 0.807007 0.149281 0.164356 11.00000 0.03104 0.02751 =
0.02091 0.00124 0.00713 -0.00550
C4 1 0.762471 0.119613 0.098186 11.00000 0.02588 0.02704 =
0.02637 0.00802 0.01121 0.00592
C1 1 0.808645 -0.226326 0.032753 11.00000 0.02334 0.02792 =
0.02190 0.00255 0.00619 0.00563
C2 1 0.806752 -0.222451 0.112604 11.00000 0.02564 0.02556 =
0.02207 0.00421 0.00860 0.00205
MOLE 2
N1 4 0.690512 0.252562 0.206834 11.00000 0.03382 0.03624 =
0.02094 -0.00046 0.01055 -0.00001
AFIX 137
H1A 2 0.695471 0.219030 0.248925 11.00000 -1.50000
H1B 2 0.698896 0.322218 0.214049 11.00000 -1.50000
H1C 2 0.709025 0.221422 0.181484 11.00000 -1.50000
AFIX 0
C5 1 0.636810 0.244161 0.166450 11.00000 0.02704 0.03414 =
0.01958 0.00370 0.00448 0.00168
AFIX 13
H5 2 0.631793 0.284891 0.121544 11.00000 -1.20000
AFIX 0
C6 1 0.622375 0.127075 0.147970 11.00000 0.03521 0.03262 =
0.03180 -0.00072 0.00930 -0.00271
AFIX 23
H6A 2 0.629238 0.084148 0.191576 11.00000 -1.20000
H6B 2 0.641945 0.098031 0.117762 11.00000 -1.20000
AFIX 0
C7 1 0.567526 0.119198 0.108945 11.00000 0.04003 0.05082 =
0.04055 -0.00609 0.00392 -0.00718
AFIX 23
H7A 2 0.561618 0.154806 0.062690 11.00000 -1.20000
H7B 2 0.558447 0.043338 0.100499 11.00000 -1.20000
AFIX 0
C8 1 0.535155 0.171030 0.151201 11.00000 0.02567 0.07907 =
0.03929 -0.00310 0.00199 -0.01165
AFIX 23
H8A 2 0.500776 0.168542 0.123208 11.00000 -1.20000
H8B 2 0.538040 0.130305 0.195057 11.00000 -1.20000
AFIX 0
C9 1 0.550189 0.287865 0.169573 11.00000 0.03257 0.06282 =
0.04552 -0.00597 0.00607 0.00837
AFIX 23
H9A 2 0.530336 0.317931 0.199056 11.00000 -1.20000
H9B 2 0.543960 0.330340 0.125827 11.00000 -1.20000
AFIX 0
C10 1 0.604963 0.295306 0.209751 11.00000 0.03185 0.03694 =
0.03348 -0.00675 0.00591 0.00223
AFIX 23
H10A 2 0.614206 0.370939 0.219018 11.00000 -1.20000
H10B 2 0.610644 0.258408 0.255545 11.00000 -1.20000
AFIX 0
MOLE 3
N2 4 0.786651 0.479802 0.088739 11.00000 0.02581 0.03139 =
0.01953 -0.00060 0.00476 -0.00067
AFIX 137
H2A 2 0.790977 0.551360 0.093099 11.00000 -1.50000
H2B 2 0.769369 0.457088 0.118471 11.00000 -1.50000
H2C 2 0.770205 0.463791 0.043799 11.00000 -1.50000
AFIX 0
C11 1 0.835937 0.424766 0.106921 11.00000 0.02324 0.02647 =
0.02059 0.00112 0.00238 0.00247
AFIX 13
H11 2 0.830691 0.346926 0.097149 11.00000 -1.20000
AFIX 0
C12 1 0.861131 0.439644 0.186658 11.00000 0.02881 0.03581 =
0.01868 0.00260 0.00551 -0.00339
AFIX 23
H12A 2 0.864657 0.516566 0.197748 11.00000 -1.20000
H12B 2 0.840604 0.407951 0.214600 11.00000 -1.20000
AFIX 0
C13 1 0.911789 0.386254 0.207061 11.00000 0.02919 0.05713 =
0.02596 0.00901 0.00275 0.00179
AFIX 23
H13A 2 0.927650 0.399667 0.257396 11.00000 -1.20000
H13B 2 0.907982 0.308347 0.200219 11.00000 -1.20000
AFIX 0
C14 1 0.944326 0.429793 0.162101 11.00000 0.02774 0.07043 =
0.03456 -0.00115 0.00294 0.00217
AFIX 23
H14A 2 0.975761 0.391484 0.174347 11.00000 -1.20000
H14B 2 0.950972 0.506222 0.172645 11.00000 -1.20000
AFIX 0
C15 1 0.919166 0.415690 0.081948 11.00000 0.02466 0.05932 =
0.03711 -0.00147 0.01315 0.00752
AFIX 23
H15A 2 0.939738 0.448072 0.054324 11.00000 -1.20000
H15B 2 0.915877 0.338862 0.070499 11.00000 -1.20000
AFIX 0
C16 1 0.867922 0.468805 0.061001 11.00000 0.03118 0.04130 =
0.02312 0.00020 0.00962 -0.00060
AFIX 23
H16A 2 0.871406 0.546851 0.067316 11.00000 -1.20000
H16B 2 0.851975 0.454413 0.010818 11.00000 -1.20000
AFIX 0
MOLE 4
N3 4 0.832374 0.186982 0.365048 11.00000 0.02739 0.03398 =
0.02073 -0.00124 0.00567 -0.00307
AFIX 137
H3A 2 0.818194 0.141475 0.329761 11.00000 -1.50000
H3B 2 0.817172 0.251092 0.357250 11.00000 -1.50000
H3C 2 0.829911 0.160118 0.406666 11.00000 -1.50000
AFIX 0
C17 1 0.885780 0.200837 0.367505 11.00000 0.02354 0.03542 =
0.02931 0.00160 0.00882 -0.00615
AFIX 13
H17 2 0.887546 0.243413 0.325454 11.00000 -1.20000
AFIX 0
C18 1 0.911436 0.264546 0.433623 11.00000 0.03259 0.05963 =
0.03389 -0.00016 0.00502 -0.01217
AFIX 23
H18A 2 0.907953 0.226856 0.476038 11.00000 -1.20000
H18B 2 0.896066 0.335451 0.432119 11.00000 -1.20000
AFIX 0
C19 1 0.966272 0.278027 0.437739 11.00000 0.03046 0.07223 =
0.05715 0.00577 -0.00110 -0.02009
AFIX 23
H19A 2 0.969693 0.322049 0.397752 11.00000 -1.20000
H19B 2 0.982731 0.315546 0.481774 11.00000 -1.20000
AFIX 0
C20 1 0.990690 0.169787 0.435763 11.00000 0.02332 0.08409 =
0.12415 0.03854 0.00163 -0.00072
AFIX 23
H20A 2 0.989569 0.127640 0.477667 11.00000 -1.20000
H20B 2 1.025197 0.180510 0.436733 11.00000 -1.20000
AFIX 0
C21 1 0.964110 0.107961 0.367679 11.00000 0.04218 0.05697 =
0.16926 0.00236 0.04905 0.01140
AFIX 23
H21A 2 0.967386 0.147854 0.325950 11.00000 -1.20000
H21B 2 0.979596 0.037483 0.367579 11.00000 -1.20000
AFIX 0
C22 1 0.909223 0.092551 0.363033 11.00000 0.03636 0.04920 =
0.08512 -0.00439 0.02276 0.00276
AFIX 23
H22A 2 0.892731 0.057401 0.318099 11.00000 -1.20000
H22B 2 0.905678 0.046447 0.402022 11.00000 -1.20000
AFIX 0
MOLE 5
CL3 3 0.766560 -0.008553 0.283681 11.00000 0.03000 0.03385 =
0.03029 -0.00566 0.01264 -0.00635
O9 5 0.801561 0.399858 0.358497 11.00000 0.03386 0.04234 =
0.02967 0.00727 0.00906 0.00336
AFIX 3
H1O 2 0.780432 0.429116 0.319544 11.00000 -1.20000
H2O 2 0.791132 0.407516 0.396547 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1210b10
REM R1 = 0.0490 for 6022 Fo > 4sig(Fo) and 0.0674 for all 7264 data
REM 346 parameters refined using 0 restraints
END
WGHT 0.0000 39.7537
REM Highest difference peak 0.658, deepest hole -0.696, 1-sigma level 0.105
Q1 1 0.8199 0.0254 0.0871 11.00000 0.05 0.66
Q2 1 0.8680 0.1239 0.2006 11.00000 0.05 0.65
Q3 1 0.7792 -0.0632 0.3108 11.00000 0.05 0.63
Q4 1 0.8323 0.0434 0.1015 11.00000 0.05 0.56
Q5 1 0.7517 0.0704 0.0681 11.00000 0.05 0.49
;
_shelxl_version_number .2013
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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 Sn 0.84481(2) -0.01264(2) 0.08670(2) 0.02266(7) Uani d 1
O O1 0.82137(11) -0.1343(2) 0.00914(14) 0.0275(6) Uani d 1
O O2 0.81693(10) -0.1304(2) 0.14399(14) 0.0247(6) Uani d 1
O O3 0.79899(11) -0.3092(2) -0.00137(15) 0.0313(6) Uani d 1
O O4 0.79534(11) -0.3041(2) 0.14046(14) 0.0307(6) Uani d 1
O O5 0.84818(10) 0.0972(2) 0.16821(14) 0.0277(6) Uani d 1
O O6 0.77157(10) 0.0445(2) 0.05761(14) 0.0273(6) Uani d 1
O O8 0.72353(11) 0.1682(3) 0.08902(16) 0.0366(7) Uani d 1
O O7 0.80129(12) 0.2174(2) 0.20695(15) 0.0332(7) Uani d 1
Cl Cl1 0.92508(4) -0.08025(10) 0.13280(7) 0.0418(3) Uani d 1
Cl Cl2 0.86238(5) 0.10594(10) 0.00174(6) 0.0429(3) Uani d 1
C C3 0.80701(16) 0.1493(3) 0.1644(2) 0.0265(8) Uani d 1
C C4 0.76247(15) 0.1196(3) 0.0982(2) 0.0256(8) Uani d 1
C C1 0.80865(15) -0.2263(3) 0.0328(2) 0.0244(8) Uani d 1
C C2 0.80675(15) -0.2225(3) 0.1126(2) 0.0240(8) Uani d 1
N N1 0.69051(13) 0.2526(3) 0.20683(17) 0.0297(8) Uani d 1
H H1A 0.6955 0.2190 0.2489 0.045 Uiso calc 1
H H1B 0.6989 0.3222 0.2140 0.045 Uiso calc 1
H H1C 0.7090 0.2214 0.1815 0.045 Uiso calc 1
C C5 0.63681(15) 0.2442(3) 0.1665(2) 0.0273(8) Uani d 1
H H5 0.6318 0.2849 0.1215 0.033 Uiso calc 1
C C6 0.62238(16) 0.1271(3) 0.1480(2) 0.0331(9) Uani d 1
H H6A 0.6292 0.0841 0.1916 0.040 Uiso calc 1
H H6B 0.6419 0.0980 0.1178 0.040 Uiso calc 1
C C7 0.56753(18) 0.1192(4) 0.1089(3) 0.0451(12) Uani d 1
H H7A 0.5616 0.1548 0.0627 0.054 Uiso calc 1
H H7B 0.5584 0.0433 0.1005 0.054 Uiso calc 1
C C8 0.53516(18) 0.1710(5) 0.1512(3) 0.0493(13) Uani d 1
H H8A 0.5008 0.1685 0.1232 0.059 Uiso calc 1
H H8B 0.5380 0.1303 0.1951 0.059 Uiso calc 1
C C9 0.55019(18) 0.2879(4) 0.1696(3) 0.0478(13) Uani d 1
H H9A 0.5303 0.3179 0.1991 0.057 Uiso calc 1
H H9B 0.5440 0.3303 0.1258 0.057 Uiso calc 1
C C10 0.60496(16) 0.2953(4) 0.2098(2) 0.0346(10) Uani d 1
H H10A 0.6142 0.3709 0.2190 0.042 Uiso calc 1
H H10B 0.6106 0.2584 0.2555 0.042 Uiso calc 1
N N2 0.78665(12) 0.4798(3) 0.08874(16) 0.0258(7) Uani d 1
H H2A 0.7910 0.5514 0.0931 0.039 Uiso calc 1
H H2B 0.7694 0.4571 0.1185 0.039 Uiso calc 1
H H2C 0.7702 0.4638 0.0438 0.039 Uiso calc 1
C C11 0.83594(14) 0.4248(3) 0.10692(19) 0.0241(8) Uani d 1
H H11 0.8307 0.3469 0.0971 0.029 Uiso calc 1
C C12 0.86113(15) 0.4396(3) 0.1867(2) 0.0279(9) Uani d 1
H H12A 0.8647 0.5166 0.1977 0.034 Uiso calc 1
H H12B 0.8406 0.4080 0.2146 0.034 Uiso calc 1
C C13 0.91179(16) 0.3863(4) 0.2071(2) 0.0383(11) Uani d 1
H H13A 0.9277 0.3997 0.2574 0.046 Uiso calc 1
H H13B 0.9080 0.3083 0.2002 0.046 Uiso calc 1
C C14 0.94433(17) 0.4298(5) 0.1621(2) 0.0453(12) Uani d 1
H H14A 0.9758 0.3915 0.1743 0.054 Uiso calc 1
H H14B 0.9510 0.5062 0.1726 0.054 Uiso calc 1
C C15 0.91917(16) 0.4157(4) 0.0819(2) 0.0394(11) Uani d 1
H H15A 0.9397 0.4481 0.0543 0.047 Uiso calc 1
H H15B 0.9159 0.3389 0.0705 0.047 Uiso calc 1
C C16 0.86792(15) 0.4688(4) 0.0610(2) 0.0314(9) Uani d 1
H H16A 0.8714 0.5469 0.0673 0.038 Uiso calc 1
H H16B 0.8520 0.4544 0.0108 0.038 Uiso calc 1
N N3 0.83237(12) 0.1870(3) 0.36505(17) 0.0275(7) Uani d 1
H H3A 0.8182 0.1415 0.3298 0.041 Uiso calc 1
H H3B 0.8172 0.2511 0.3573 0.041 Uiso calc 1
H H3C 0.8299 0.1601 0.4067 0.041 Uiso calc 1
C C17 0.88578(15) 0.2008(3) 0.3675(2) 0.0291(9) Uani d 1
H H17 0.8875 0.2434 0.3255 0.035 Uiso calc 1
C C18 0.91144(17) 0.2645(4) 0.4336(2) 0.0428(12) Uani d 1
H H18A 0.9080 0.2269 0.4760 0.051 Uiso calc 1
H H18B 0.8961 0.3355 0.4321 0.051 Uiso calc 1
C C19 0.96627(18) 0.2780(5) 0.4377(3) 0.0557(15) Uani d 1
H H19A 0.9697 0.3220 0.3978 0.067 Uiso calc 1
H H19B 0.9827 0.3155 0.4818 0.067 Uiso calc 1
C C20 0.9907(2) 0.1698(6) 0.4358(4) 0.081(2) Uani d 1
H H20A 0.9896 0.1276 0.4777 0.097 Uiso calc 1
H H20B 1.0252 0.1805 0.4367 0.097 Uiso calc 1
C C21 0.9641(2) 0.1080(5) 0.3677(5) 0.085(2) Uani d 1
H H21A 0.9674 0.1479 0.3259 0.103 Uiso calc 1
H H21B 0.9796 0.0375 0.3676 0.103 Uiso calc 1
C C22 0.90922(19) 0.0926(4) 0.3630(4) 0.0556(15) Uani d 1
H H22A 0.8927 0.0574 0.3181 0.067 Uiso calc 1
H H22B 0.9057 0.0464 0.4020 0.067 Uiso calc 1
Cl Cl3 0.76656(4) -0.00855(8) 0.28368(5) 0.0305(2) Uani d 1
O O9 0.80156(11) 0.3999(2) 0.35850(16) 0.0352(7) Uani d 1
H H1O 0.7804 0.4291 0.3195 0.042 Uiso d 1
H H2O 0.7911 0.4075 0.3965 0.042 Uiso d 1
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
Sn 0.02068(13) 0.02730(13) 0.01990(12) -0.00111(11) 0.00525(9) 0.00308(11)
O1 0.0342(16) 0.0295(14) 0.0206(13) -0.0004(12) 0.0103(12) 0.0007(11)
O2 0.0285(15) 0.0254(13) 0.0212(13) -0.0018(11) 0.0086(11) 0.0002(11)
O3 0.0387(18) 0.0303(15) 0.0258(15) 0.0031(13) 0.0102(13) -0.0038(12)
O4 0.0421(18) 0.0279(14) 0.0241(14) -0.0028(13) 0.0124(13) 0.0019(12)
O5 0.0299(16) 0.0276(14) 0.0259(14) 0.0022(12) 0.0082(12) 0.0016(11)
O6 0.0253(15) 0.0298(14) 0.0228(13) 0.0025(11) -0.0007(11) -0.0039(11)
O8 0.0314(17) 0.0458(18) 0.0323(16) 0.0102(14) 0.0080(13) -0.0029(14)
O7 0.0456(19) 0.0305(15) 0.0239(14) -0.0047(13) 0.0102(13) -0.0057(12)
Cl1 0.0225(5) 0.0539(7) 0.0497(7) 0.0053(5) 0.0107(5) 0.0141(5)
Cl2 0.0541(7) 0.0439(6) 0.0339(6) -0.0059(5) 0.0175(5) 0.0134(5)
C3 0.031(2) 0.0275(19) 0.0209(19) -0.0055(16) 0.0071(17) 0.0012(16)
C4 0.026(2) 0.0270(19) 0.026(2) 0.0059(16) 0.0112(17) 0.0080(16)
C1 0.023(2) 0.0279(19) 0.0219(19) 0.0056(16) 0.0062(16) 0.0025(15)
C2 0.026(2) 0.0256(19) 0.0221(19) 0.0021(15) 0.0086(16) 0.0042(15)
N1 0.034(2) 0.0362(19) 0.0209(16) 0.0000(15) 0.0105(15) -0.0005(14)
C5 0.027(2) 0.034(2) 0.0196(19) 0.0017(17) 0.0045(16) 0.0037(16)
C6 0.035(2) 0.033(2) 0.032(2) -0.0027(18) 0.0093(19) -0.0007(18)
C7 0.040(3) 0.051(3) 0.041(3) -0.007(2) 0.004(2) -0.006(2)
C8 0.026(2) 0.079(4) 0.039(3) -0.012(2) 0.002(2) -0.003(3)
C9 0.033(3) 0.063(3) 0.046(3) 0.008(2) 0.006(2) -0.006(2)
C10 0.032(2) 0.037(2) 0.033(2) 0.0022(19) 0.0059(19) -0.0068(19)
N2 0.0258(17) 0.0314(17) 0.0195(15) -0.0007(14) 0.0048(13) -0.0006(14)
C11 0.023(2) 0.0265(19) 0.0206(18) 0.0025(15) 0.0024(15) 0.0011(15)
C12 0.029(2) 0.036(2) 0.0187(18) -0.0034(17) 0.0055(16) 0.0026(16)
C13 0.029(2) 0.057(3) 0.026(2) 0.002(2) 0.0027(18) 0.009(2)
C14 0.028(2) 0.070(3) 0.035(2) 0.002(2) 0.003(2) -0.001(2)
C15 0.025(2) 0.059(3) 0.037(2) 0.008(2) 0.0132(19) -0.001(2)
C16 0.031(2) 0.041(2) 0.0231(19) -0.0006(19) 0.0096(17) 0.0002(17)
N3 0.0274(18) 0.0340(18) 0.0207(16) -0.0031(14) 0.0057(14) -0.0012(14)
C17 0.024(2) 0.035(2) 0.029(2) -0.0061(17) 0.0088(17) 0.0016(17)
C18 0.033(3) 0.060(3) 0.034(2) -0.012(2) 0.005(2) 0.000(2)
C19 0.030(3) 0.072(4) 0.057(3) -0.020(3) -0.001(2) 0.006(3)
C20 0.023(3) 0.084(5) 0.124(6) -0.001(3) 0.002(3) 0.039(5)
C21 0.042(4) 0.057(4) 0.169(8) 0.011(3) 0.049(5) 0.002(5)
C22 0.036(3) 0.049(3) 0.085(4) 0.003(2) 0.023(3) -0.004(3)
Cl3 0.0300(5) 0.0338(5) 0.0303(5) -0.0063(4) 0.0126(4) -0.0057(4)
O9 0.0339(17) 0.0423(17) 0.0297(15) 0.0034(14) 0.0091(13) 0.0073(13)
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'
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
O5 Sn O6 79.99(10)
O5 Sn O1 163.31(11)
O6 Sn O1 87.22(10)
O5 Sn O2 89.79(10)
O6 Sn O2 84.16(11)
O1 Sn O2 78.19(10)
O5 Sn Cl1 95.71(8)
O6 Sn Cl1 173.10(8)
O1 Sn Cl1 95.93(8)
O2 Sn Cl1 90.46(8)
O5 Sn Cl2 98.78(8)
O6 Sn Cl2 88.65(8)
O1 Sn Cl2 91.55(8)
O2 Sn Cl2 167.72(8)
Cl1 Sn Cl2 97.37(4)
C1 O1 Sn 115.6(2)
C2 O2 Sn 115.3(2)
C3 O5 Sn 114.9(2)
C4 O6 Sn 114.7(2)
O7 C3 O5 125.1(4)
O7 C3 C4 119.5(4)
O5 C3 C4 115.4(3)
O8 C4 O6 125.7(4)
O8 C4 C3 119.3(4)
O6 C4 C3 115.0(3)
O3 C1 O1 125.8(4)
O3 C1 C2 120.4(3)
O1 C1 C2 113.9(3)
O4 C2 O2 124.7(3)
O4 C2 C1 119.6(3)
O2 C2 C1 115.7(3)
C5 N1 H1A 109.5
C5 N1 H1B 109.5
H1A N1 H1B 109.5
C5 N1 H1C 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
N1 C5 C6 110.8(3)
N1 C5 C10 109.8(3)
C6 C5 C10 111.5(4)
N1 C5 H5 108.2
C6 C5 H5 108.2
C10 C5 H5 108.2
C5 C6 C7 110.4(4)
C5 C6 H6A 109.6
C7 C6 H6A 109.6
C5 C6 H6B 109.6
C7 C6 H6B 109.6
H6A C6 H6B 108.1
C8 C7 C6 112.0(4)
C8 C7 H7A 109.2
C6 C7 H7A 109.2
C8 C7 H7B 109.2
C6 C7 H7B 109.2
H7A C7 H7B 107.9
C9 C8 C7 111.0(4)
C9 C8 H8A 109.4
C7 C8 H8A 109.4
C9 C8 H8B 109.4
C7 C8 H8B 109.4
H8A C8 H8B 108.0
C8 C9 C10 110.8(4)
C8 C9 H9A 109.5
C10 C9 H9A 109.5
C8 C9 H9B 109.5
C10 C9 H9B 109.5
H9A C9 H9B 108.1
C5 C10 C9 110.7(4)
C5 C10 H10A 109.5
C9 C10 H10A 109.5
C5 C10 H10B 109.5
C9 C10 H10B 109.5
H10A C10 H10B 108.1
C11 N2 H2A 109.5
C11 N2 H2B 109.5
H2A N2 H2B 109.5
C11 N2 H2C 109.5
H2A N2 H2C 109.5
H2B N2 H2C 109.5
N2 C11 C16 110.6(3)
N2 C11 C12 109.4(3)
C16 C11 C12 111.3(3)
N2 C11 H11 108.5
C16 C11 H11 108.5
C12 C11 H11 108.5
C13 C12 C11 111.0(3)
C13 C12 H12A 109.4
C11 C12 H12A 109.4
C13 C12 H12B 109.4
C11 C12 H12B 109.4
H12A C12 H12B 108.0
C14 C13 C12 111.2(4)
C14 C13 H13A 109.4
C12 C13 H13A 109.4
C14 C13 H13B 109.4
C12 C13 H13B 109.4
H13A C13 H13B 108.0
C13 C14 C15 110.9(4)
C13 C14 H14A 109.5
C15 C14 H14A 109.5
C13 C14 H14B 109.5
C15 C14 H14B 109.5
H14A C14 H14B 108.0
C16 C15 C14 111.4(4)
C16 C15 H15A 109.4
C14 C15 H15A 109.4
C16 C15 H15B 109.4
C14 C15 H15B 109.4
H15A C15 H15B 108.0
C11 C16 C15 110.5(3)
C11 C16 H16A 109.6
C15 C16 H16A 109.6
C11 C16 H16B 109.6
C15 C16 H16B 109.6
H16A C16 H16B 108.1
C17 N3 H3A 109.5
C17 N3 H3B 109.5
H3A N3 H3B 109.5
C17 N3 H3C 109.5
H3A N3 H3C 109.5
H3B N3 H3C 109.5
N3 C17 C22 110.3(3)
N3 C17 C18 109.4(3)
C22 C17 C18 113.3(4)
N3 C17 H17 107.9
C22 C17 H17 107.9
C18 C17 H17 107.9
C17 C18 C19 110.2(4)
C17 C18 H18A 109.6
C19 C18 H18A 109.6
C17 C18 H18B 109.6
C19 C18 H18B 109.6
H18A C18 H18B 108.1
C20 C19 C18 111.1(5)
C20 C19 H19A 109.4
C18 C19 H19A 109.4
C20 C19 H19B 109.4
C18 C19 H19B 109.4
H19A C19 H19B 108.0
C19 C20 C21 110.1(5)
C19 C20 H20A 109.6
C21 C20 H20A 109.6
C19 C20 H20B 109.6
C21 C20 H20B 109.6
H20A C20 H20B 108.2
C22 C21 C20 111.2(6)
C22 C21 H21A 109.4
C20 C21 H21A 109.4
C22 C21 H21B 109.4
C20 C21 H21B 109.4
H21A C21 H21B 108.0
C17 C22 C21 109.6(4)
C17 C22 H22A 109.8
C21 C22 H22A 109.8
C17 C22 H22B 109.8
C21 C22 H22B 109.8
H22A C22 H22B 108.2
H1O O9 H2O 111.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn O5 2.060(3)
Sn O6 2.097(3)
Sn O1 2.097(3)
Sn O2 2.098(3)
Sn Cl1 2.3370(11)
Sn Cl2 2.3466(10)
O1 C1 1.306(5)
O2 C2 1.281(5)
O3 C1 1.206(5)
O4 C2 1.222(4)
O5 C3 1.303(5)
O6 C4 1.282(5)
O8 C4 1.214(5)
O7 C3 1.215(5)
C3 C4 1.572(6)
C1 C2 1.561(5)
N1 C5 1.500(5)
N1 H1A 0.8900
N1 H1B 0.8900
N1 H1C 0.8900
C5 C6 1.513(6)
C5 C10 1.514(6)
C5 H5 0.9800
C6 C7 1.522(6)
C6 H6A 0.9700
C6 H6B 0.9700
C7 C8 1.514(7)
C7 H7A 0.9700
C7 H7B 0.9700
C8 C9 1.514(7)
C8 H8A 0.9700
C8 H8B 0.9700
C9 C10 1.525(6)
C9 H9A 0.9700
C9 H9B 0.9700
C10 H10A 0.9700
C10 H10B 0.9700
N2 C11 1.492(5)
N2 H2A 0.8900
N2 H2B 0.8900
N2 H2C 0.8900
C11 C16 1.520(5)
C11 C12 1.526(5)
C11 H11 0.9800
C12 C13 1.516(6)
C12 H12A 0.9700
C12 H12B 0.9700
C13 C14 1.516(6)
C13 H13A 0.9700
C13 H13B 0.9700
C14 C15 1.531(6)
C14 H14A 0.9700
C14 H14B 0.9700
C15 C16 1.529(6)
C15 H15A 0.9700
C15 H15B 0.9700
C16 H16A 0.9700
C16 H16B 0.9700
N3 C17 1.493(5)
N3 H3A 0.8900
N3 H3B 0.8900
N3 H3C 0.8900
C17 C22 1.498(6)
C17 C18 1.508(6)
C17 H17 0.9800
C18 C19 1.524(7)
C18 H18A 0.9700
C18 H18B 0.9700
C19 C20 1.503(9)
C19 H19A 0.9700
C19 H19B 0.9700
C20 C21 1.530(10)
C20 H20A 0.9700
C20 H20B 0.9700
C21 C22 1.526(7)
C21 H21A 0.9700
C21 H21B 0.9700
C22 H22A 0.9700
C22 H22B 0.9700
O9 H1O 0.8992
O9 H2O 0.8667
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 H1A O4 4_655 0.89 2.11 2.957(4) 159.9
N1 H1B Cl3 4_655 0.89 2.29 3.163(4) 166.1
N1 H1C O8 . 0.89 2.05 2.873(4) 154.3
N1 H1C O7 . 0.89 2.50 3.130(5) 128.6
N2 H2A O4 1_565 0.89 1.99 2.829(4) 156.7
N2 H2A O3 1_565 0.89 2.56 3.197(4) 129.2
N2 H2B Cl3 4_655 0.89 2.41 3.209(3) 150.1
N2 H2C O6 7_655 0.89 2.00 2.879(4) 169.5
N3 H3A Cl3 . 0.89 2.37 3.180(3) 151.8
N3 H3A O7 . 0.89 2.48 2.971(4) 115.4
N3 H3B O9 . 0.89 1.88 2.751(5) 164.0
N3 H3C O1 6_556 0.89 2.08 2.957(4) 166.8
O9 H1O Cl3 4_655 0.90 2.21 3.108(3) 173.4
O9 H2O O3 6_556 0.87 2.28 2.950(4) 134.7