#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2101624.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_2101624
loop_
_publ_author_name
'Li, Q.'
'Mak, T. C. W.'
_publ_section_title
;
 Inclusion compounds of thiourea and peralkylated ammonium salts. III.
 Hydrogen-bonded host lattices built of thiourea and nitrate ions
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              989
_journal_page_last               998
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C11 H32 N8 O3 S3'
_chemical_formula_weight         420.60
_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_type_scat_source           IntTabIV
_cell_angle_alpha                75.30(3)
_cell_angle_beta                 86.98(3)
_cell_angle_gamma                72.25(3)
_cell_formula_units_Z            4
_cell_length_a                   10.300(2)
_cell_length_b                   14.704(3)
_cell_length_c                   15.784(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     2201.4(10)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7718
_diffrn_reflns_theta_max         23.5
_diffrn_standards_decay_%        +-1.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   '\y scan'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.22
_refine_ls_goodness_of_fit_obs   1.52
_refine_ls_hydrogen_treatment    'H atoms refined using a riding model'
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5034
_refine_ls_R_factor_obs          0.039
_refine_ls_shift/esd_max         0.012
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(F~o~) + 0.0003|F~o~|^2^]'
_refine_ls_wR_factor_obs         0.049
_reflns_number_observed          5034
_reflns_number_total             6464
_reflns_observed_criterion       |F~o~|>3\s(|F~o~|)
_[local]_cod_data_source_file    cr0511.cif
_[local]_cod_data_source_block   cr0511a
_cod_original_cell_volume        2201.5(7)
_cod_database_code               2101624
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
S(1) .59870(10) .44700(10) .13630(10) .0710(10)
C(1) .7001(2) .4761(2) .19950(10) .0450(10)
N(1) .8320(2) .42630(10) .21290(10) .0540(10)
N(2) .6501(2) .55010(10) .23870(10) .0530(10)
S(2) .32190(10) .69770(10) .19840(10) .0500(10)
C(2) .2763(2) .7191(2) .0911(2) .0420(10)
N(3) .3312(2) .65230(10) .04620(10) .0560(10)
N(4) .1849(2) .80270(10) .05110(10) .0550(10)
S(3) .03910(10) .97220(10) .17050(10) .0650(10)
C(3) .1704(2) .9867(2) .2207(2) .0480(10)
N(5) .1509(2) 1.0618(2) .25820(10) .0610(10)
N(6) .2960(2) .9258(2) .22400(10) .0610(10)
S(4) -.07750(10) .53620(10) .36140(10) .0490(10)
C(4) .0337(2) .5863(2) .29700(10) .0410(10)
N(7) .1473(2) .53040(10) .26970(10) .0520(10)
N(8) .0094(2) .68410(10) .27290(10) .0520(10)
S(5) .19420(10) .28060(10) .31640(10) .0500(10)
C(5) .2332(2) .2629(2) .42410(10) .0380(10)
N(9) .1771(2) .33200(10) .46690(10) .0490(10)
N(10) .3210(2) .17910(10) .46830(10) .0500(10)
S(6) .47000(10) -.00170(10) .36000(10) .0430(10)
C(6) .5687(2) .0592(2) .29280(10) .0390(10)
N(11) .6881(2) .01030(10) .26740(10) .0540(10)
N(12) .5276(2) .15780(10) .26510(10) .0490(10)
N(15) .8327(2) .20880(10) .17200(10) .0470(10)
O(1) .8450(2) .18500(10) .25300(10) .0630(10)
O(2) .9078(2) .25200(10) .12530(10) .0640(10)
O(3) .7415(2) .18970(10) .13610(10) .0580(10)
N(16) -.3440(2) .76700(10) .31760(10) .0470(10)
O(4) -.3739(2) .7843(2) .24100(10) .0990(10)
O(5) -.4031(2) .7239(2) .37560(10) .0830(10)
O(6) -.2474(2) .79360(10) .34050(10) .0510(10)
N(13) .2486(2) .74720(10) .50660(10) .0430(10)
C(7) .0962(2) .7747(2) .5155(2) .0710(10)
C(8) .0155(3) .8407(2) .4318(2) .0940(10)
C(9) .3110(2) .6859(2) .5962(2) .0630(10)
C(10) .4640(3) .6507(2) .6016(2) .0880(10)
C(11) .2950(2) .8383(2) .4771(2) .0580(10)
C(12) .2484(3) .9112(2) .5339(2) 7.090(10)
C(13) .2951(2) .6890(2) .4382(2) .0640(10)
C(14) .2666(3) .5894(2) .4586(2) .0790(10)
N(14) .2594(2) .24360(10) .00090(10) .0460(10)
C(15) .4037(2) .2136(2) -.0316(2) .0650(10)
C(16) .5032(2) .1277(2) .0296(2) .0850(10)
C(17) .2564(2) .2726(2) .0870(2) .0550(10)
C(18) .3144(3) .3558(2) .0851(2) .0800(10)
C(19) .1785(2) .3305(2) -.0704(2) .0610(10)
C(20) .0306(2) .3742(2) -.0516(2) .0790(10)
C(21) .1984(2) .1588(2) .0178(2) .0520(10)
C(22) .1892(2) .1197(2) -.0612(2) .0700(10)
H(1A) .8708 .3760 .1881 .080
H(1B) .8826 .4436 .2472 .080
H(2A) .5614 .5856 .2314 .080
H(2B) .7054 .5642 .2723 .080
H(3A) .3931 .5951 .0723 .080
H(3B) .3063 .6642 -.0103 .080
H(4A) .1465 .8493 .0801 .080
H(4B) .1616 .8129 -.0055 .080
H(5A) .0673 1.1052 .2571 .080
H(5B) .2214 1.0689 .2846 .080
H(6A) .3141 .8744 .1995 .080
H(6B) .3633 .9358 .2511 .080
H(7A) .1662 .4643 .2855 .080
H(7B) .2049 .5580 .2357 .080
H(8A) -.0660 .7237 .2910 .080
H(8B) .0683 .7103 .2388 .080
H(9A) .1182 .3897 .4387 .080
H(9B) .1989 .3214 .5238 .080
H(10A) .3602 .1310 .4410 .080
H(10B) .3410 .1704 .5252 .080
H(11A) .7181 -.0559 .2858 .080
H(11B) .7394 .0430 .2320 .080
H(12A) .4475 .1927 .2826 .080
H(12B) .5803 .1892 .2297 .080
H(7C) .0717 .8083 .5615 .100
H(7D) .0697 .7155 .5324 .100
H(8C) -.0806 .8558 .4417 .120
H(8D) .0399 .9008 .4151 .120
H(8E) .0379 .8071 .3857 .120
H(9C) .2781 .6296 .6128 .080
H(9D) .2791 .7243 .6382 .080
H(10C) .4936 .6127 .6601 .100
H(10D) .4976 .6103 .5613 .100
H(10E) .4986 .7063 .5870 .100
H(11C) .2635 .8711 .4178 .080
H(11D) .3928 .8178 .4779 .080
H(12C) .2816 .9669 .5124 .100
H(12D) .1505 .9330 .5324 .100
H(12E) .2812 .8792 .5931 .100
H(13A) .3913 .6781 .4312 .100
H(13B) .2505 .7275 .3831 .100
H(14A) .2992 .5565 .4128 .120
H(14B) .3127 .5496 .5129 .120
H(14C) .1703 .5996 .4642 .120
H(15A) .4382 .2691 -.0418 .100
H(15B) .4000 .1984 -.0870 .100
H(16A) .5910 .1144 .0033 .120
H(16B) .5105 .1425 .0847 .120
H(16C) .4718 .0709 .0390 .120
H(17A) .3067 .2154 .1302 .080
H(17B) .1637 .2911 .1054 .080
H(18A) .3093 .3686 .1421 .100
H(18B) .4079 .3374 .0684 .100
H(18C) .2633 .4140 .0433 .100
H(19A) .1813 .3093 -.1234 .080
H(19B) .2219 .3814 -.0811 .080
H(20A) -.0138 .4283 -.0994 .100
H(20B) -.0145 .3243 -.0422 .100
H(20C) .0265 .3972 .0005 .100
H(21A) .1085 .1802 .0398 .080
H(21B) .2525 .1054 .0627 .080
H(22A) .1497 .0666 -.0449 .100
H(22B) .1332 .1720 -.1060 .100
H(22C) .2789 .0963 -.0829 .100
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
S(1) C(1) N(1) 121.6(2) yes
N(1) C(1) N(2) 117.3(3) yes
S(2) C(2) N(3) 120.6(2) yes
N(3) C(2) N(4) 118.7(2) yes
S(3) C(3) N(5) 120.8(2) yes
N(5) C(3) N(6) 117.1(3) yes
S(4) C(4) N(7) 121.7(2) yes
N(7) C(4) N(8) 117.9(2) yes
S(5) C(5) N(9) 121.30(10) yes
N(9) C(5) N(10) 117.8(2) yes
S(6) C(6) N(11) 120.8(2) yes
N(11) C(6) N(12) 118.3(2) yes
C(7) N(13) C(9) 106.9(2) no
C(9) N(13) C(11) 110.9(2) no
S(1) C(1) N(2) 121.1(2) yes
S(2) C(2) N(4) 120.6(2) yes
S(3) C(3) N(6) 122.2(3) yes
S(4) C(4) N(8) 120.4(2) yes
S(5) C(5) N(10) 120.9(2) yes
S(6) C(6) N(12) 120.9(2) yes
C(7) N(13) C(11) 110.9(2) no
C(7) N(13) C(13) 111.3(3) no
C(9) N(13) C(13) 110.5(2) no
N(13) C(7) C(8) 114.2(3) no
N(13) C(11) C(12) 114.7(2) no
C(15) N(14) C(17) 111.2(2) no
C(17) N(14) C(19) 110.7(2) no
C(17) N(14) C(21) 106.8(2) no
N(14) C(15) C(16) 115.3(2) no
N(14) C(19) C(20) 115.6(2) no
C(11) N(13) C(13) 106.4(2) no
N(13) C(9) C(10) 115.4(2) no
N(13) C(13) C(14) 115.1(3) no
C(15) N(14) C(19) 106.1(2) no
C(15) N(14) C(21) 111.1(2) no
C(19) N(14) C(21) 111.0(2) no
N(14) C(17) C(18) 115.6(2) no
N(14) C(21) C(22) 115.3(2) no
O(1) N(15) O(2) 121.4(3) yes
O(2) N(15) O(3) 119.2(2) yes
O(4) N(16) O(6) 120.0(3) yes
O(1) N(15) O(3) 119.4(2) yes
O(4) N(16) O(5) 122.4(3) yes
O(5) N(16) O(6) 117.6(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S(1) C(1) 1.693(3) yes
C(1) N(2) 1.341(4) yes
S(2) C(2) 1.707(3) yes
C(2) N(4) 1.327(3) yes
S(3) C(3) 1.697(3) yes
C(3) N(6) 1.325(3) yes
S(4) C(4) 1.703(2) yes
C(4) N(8) 1.338(3) yes
S(5) C(5) 1.704(3) yes
C(5) N(10) 1.332(2) yes
S(6) C(6) 1.709(3) yes
C(6) N(12) 1.339(3) yes
N(13) C(7) 1.505(4) no
N(13) C(11) 1.513(4) no
C(7) C(8) 1.533(5) no
C(11) C(12) 1.521(5) no
N(14) C(15) 1.517(4) no
N(14) C(19) 1.521(3) no
C(15) C(16) 1.508(4) no
C(19) C(20) 1.508(4) no
N(15) O(1) 1.240(3) yes
N(15) O(3) 1.257(4) yes
N(16) O(4) 1.207(3) yes
N(16) O(6) 1.272(4) yes
C(1) N(1) 1.331(3) yes
C(2) N(3) 1.326(4) yes
C(3) N(5) 1.341(4) yes
C(4) N(7) 1.330(3) yes
C(5) N(9) 1.330(3) yes
C(6) N(11) 1.321(3) no
N(13) C(9) 1.523(3) no
N(13) C(13) 1.514(4) no
C(9) C(10) 1.501(5) no
C(13) C(14) 1.532(5) no
N(14) C(17) 1.521(4) no
N(14) C(21) 1.520(4) no
C(17) C(18) 1.510(6) no
C(21) C(22) 1.517(5) no
N(15) O(2) 1.243(3) yes
N(16) O(5) 1.221(3) yes