#------------------------------------------------------------------------------
#$Date: 2017-05-05 08:49:52 +0300 (Fri, 05 May 2017) $
#$Revision: 196234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/40/2004068.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_2004068
loop_
_publ_author_name
'Ng, S. W.'
_publ_section_title
;
 Bis(dicyclohexylammonium) Trithiocarbodiglycolate
 Trithiocarbodiglycolic Acid
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2150
_journal_page_last               2152
_journal_paper_doi               10.1107/S010827019500312X
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C17 H29 N O4 S3'
_chemical_formula_weight         407.59
_chemical_name_systematic
;
bis(dicyclohexylammonium trithiocarbodiglycolate trithiocarbodiglycolic acid
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.315(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.664(2)
_cell_length_b                   9.829(4)
_cell_length_c                   20.058(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12
_cell_measurement_theta_min      6
_cell_volume                     2027.7(9)
_computing_cell_refinement
;
CAD-4 VAX/PC Fortran System (Enraf-Nonius, 1988)
;
_computing_data_collection
;
CAD-4 VAX/PC Fortran System (Enraf-Nonius, 1988)
;
_computing_data_reduction        'Xtal3.0 (Hall & Stewart, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution
;
MULTAN80 (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980)
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω-2θ
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7310
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       cube
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.992
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0553P)^2^ + 0.0577P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_obs         0.0999
_reflns_number_observed          2273
_reflns_number_total             3571
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1016.cif
_cod_data_source_block           ta1016
_cod_depositor_comments
;

2017-04-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H58 N2 O8 S6'
_cod_original_formula_weight         815.18
_cod_original_formula_moiety         'C34 H58 N2 O8 S6'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2027.6(9)
_cod_original_sg_symbol_H-M      'P 2/a'
_cod_database_code               2004068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z'
'-x, -y, -z'
'-x-1/2, y, -z'
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
S1A 1 0.7500 0.32840(13) 0.5000 0.0520(3) Uani d S S
S1B 1 0.7500 0.36004(13) 0 0.0631(4) Uani d S S
S2 1 0.84089(9) 0.05733(9) 0.46167(4) 0.0473(3) Uani d . S
S3 1 0.66937(9) 0.62985(9) 0.04536(4) 0.0476(2) Uani d . S
O1 1 0.8445(2) 0.3111(2) 0.31111(12) 0.0521(6) Uani d . O
O2 1 0.6960(2) 0.1604(2) 0.32197(11) 0.0498(6) Uani d . O
O3 1 0.6894(2) 0.3920(2) 0.20567(12) 0.0506(6) Uani d . O
O4 1 0.8431(2) 0.5126(2) 0.17547(11) 0.0471(6) Uani d . O
N1 1 0.4493(3) 0.2395(3) 0.24539(13) 0.0335(6) Uani d . N
C1A 1 0.7500 0.1639(4) 0.5000 0.0336(10) Uani d S C
C1B 1 0.7500 0.5247(4) 0 0.0397(11) Uani d S C
C2 1 0.9005(3) 0.1697(4) 0.4072(2) 0.0481(9) Uani d . C
H2A 1 0.9359(3) 0.2498(4) 0.4339(2) 0.072 Uiso calc R H
H2B 1 0.9717(3) 0.1250(4) 0.3942(2) 0.072 Uiso calc R H
C3 1 0.8022(3) 0.2159(3) 0.34175(15) 0.0372(8) Uani d . C
C4 1 0.6228(3) 0.5145(4) 0.1036(2) 0.0492(9) Uani d . C
H4A 1 0.5543(3) 0.5566(4) 0.1201(2) 0.074 Uiso calc R H
H4B 1 0.5866(3) 0.4334(4) 0.0782(2) 0.074 Uiso calc R H
C5 1 0.7311(3) 0.4719(3) 0.1657(2) 0.0398(8) Uani d . C
C6 1 0.3867(3) 0.2372(3) 0.30438(15) 0.0348(7) Uani d . C
H6 1 0.4104(3) 0.1516(3) 0.32967(15) 0.052 Uiso calc R H
C7 1 0.2400(3) 0.2443(4) 0.2796(2) 0.0431(8) Uani d . C
H7A 1 0.2077(3) 0.1653(4) 0.2513(2) 0.065 Uiso calc R H
H7B 1 0.2149(3) 0.3247(4) 0.2511(2) 0.065 Uiso calc R H
C8 1 0.1787(3) 0.2494(4) 0.3399(2) 0.0493(9) Uani d . C
H8A 1 0.0855(3) 0.2609(4) 0.3224(2) 0.074 Uiso calc R H
H8B 1 0.1945(3) 0.1640(4) 0.3649(2) 0.074 Uiso calc R H
C9 1 0.2339(4) 0.3654(4) 0.3888(2) 0.0625(11) Uani d . C
H9A 1 0.1974(4) 0.3624(4) 0.4282(2) 0.094 Uiso calc R H
H9B 1 0.2095(4) 0.4515(4) 0.3653(2) 0.094 Uiso calc R H
C10 1 0.3812(3) 0.3561(4) 0.4137(2) 0.0587(10) Uani d . C
H10A 1 0.4054(3) 0.2741(4) 0.4409(2) 0.088 Uiso calc R H
H10B 1 0.4146(3) 0.4335(4) 0.4430(2) 0.088 Uiso calc R H
C11 1 0.4417(3) 0.3537(3) 0.3528(2) 0.0440(8) Uani d . C
H11A 1 0.4241(3) 0.4391(3) 0.3279(2) 0.066 Uiso calc R H
H11B 1 0.5352(3) 0.3435(3) 0.3697(2) 0.066 Uiso calc R H
C12 1 0.4058(3) 0.1350(3) 0.18885(14) 0.0337(7) Uani d . C
H12 1 0.3129(3) 0.1482(3) 0.16704(14) 0.050 Uiso calc R H
C13 1 0.4260(3) -0.0075(3) 0.2179(2) 0.0465(8) Uani d . C
H13A 1 0.3705(3) -0.0221(3) 0.2485(2) 0.070 Uiso calc R H
H13B 1 0.5155(3) -0.0182(3) 0.2446(2) 0.070 Uiso calc R H
C14 1 0.3944(4) -0.1135(4) 0.1596(2) 0.0586(10) Uani d . C
H14A 1 0.4159(4) -0.2035(4) 0.1792(2) 0.088 Uiso calc R H
H14B 1 0.3019(4) -0.1116(4) 0.1373(2) 0.088 Uiso calc R H
C15 1 0.4688(4) -0.0870(4) 0.1064(2) 0.0566(10) Uani d . C
H15A 1 0.4420(4) -0.1520(4) 0.0689(2) 0.085 Uiso calc R H
H15B 1 0.5610(4) -0.0997(4) 0.1274(2) 0.085 Uiso calc R H
C16 1 0.4451(4) 0.0559(4) 0.0778(2) 0.0602(10) Uani d . C
H16A 1 0.3543(4) 0.0659(4) 0.0530(2) 0.090 Uiso calc R H
H16B 1 0.4971(4) 0.0715(4) 0.0455(2) 0.090 Uiso calc R H
C17 1 0.4801(3) 0.1605(3) 0.1355(2) 0.0438(8) Uani d . C
H17A 1 0.5727(3) 0.1563(3) 0.1574(2) 0.066 Uiso calc R H
H17B 1 0.4601(3) 0.2509(3) 0.1162(2) 0.066 Uiso calc R H
H1 1 0.7654(48) 0.3564(48) 0.2559(25) 0.120(17) Uiso d . H
H2 1 0.5503(41) 0.2308(40) 0.2668(19) 0.082(13) Uiso d . H
H3 1 0.4327(29) 0.3181(34) 0.2263(16) 0.040(9) Uiso d . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033
O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060
S S 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.1234
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1A S2 C2 . 103.2(2) yes
C1B S3 C4 . 103.0(2) yes
C6 N1 C12 . 117.9(2) yes
S1A C1A S2 . 127.04(12) yes
S1A C1A S2 4_756 127.04(12) yes
S2 C1A S2 4_756 105.9(2) yes
S1B C1B S3 . 126.28(12) yes
S1B C1B S3 4_755 126.28(12) yes
S3 C1B S3 4_755 107.4(2) yes
C3 C2 S2 . 116.0(2) yes
O2 C3 O1 . 126.1(3) yes
O2 C3 C2 . 121.0(3) yes
O1 C3 C2 . 112.8(3) yes
C5 C4 S3 . 115.4(2) yes
O4 C5 O3 . 125.8(3) yes
O4 C5 C4 . 122.7(3) yes
O3 C5 C4 . 111.5(3) yes
N1 C6 C7 . 112.1(2) yes
N1 C6 C11 . 108.4(2) yes
C7 C6 C11 . 111.5(3) yes
C6 C7 C8 . 111.3(3) yes
C9 C8 C7 . 111.4(3) yes
C8 C9 C10 . 110.9(3) yes
C9 C10 C11 . 110.9(3) yes
C6 C11 C10 . 110.6(3) yes
N1 C12 C13 . 110.9(2) yes
N1 C12 C17 . 107.7(2) yes
C13 C12 C17 . 112.2(3) yes
C12 C13 C14 . 110.9(3) yes
C15 C14 C13 . 111.7(3) yes
C14 C15 C16 . 111.2(3) yes
C15 C16 C17 . 110.9(3) yes
C12 C17 C16 . 111.0(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1A C1A . 1.617(5) yes
S1B C1B . 1.619(5) yes
S2 C1A . 1.738(3) yes
S2 C2 . 1.784(3) yes
S3 C1B . 1.746(3) yes
S3 C4 . 1.790(3) yes
O1 C3 . 1.266(4) yes
O2 C3 . 1.224(4) yes
O3 C5 . 1.283(4) yes
O4 C5 . 1.225(4) yes
N1 C6 . 1.504(4) yes
N1 C12 . 1.510(4) yes
C1A S2 4_756 1.738(3) yes
C1B S3 4_755 1.746(3) yes
C2 C3 . 1.518(4) yes
C4 C5 . 1.517(4) yes
C6 C7 . 1.513(4) yes
C6 C11 . 1.515(4) yes
C7 C8 . 1.520(4) yes
C8 C9 . 1.517(5) yes
C9 C10 . 1.521(5) yes
C10 C11 . 1.524(4) yes
C12 C13 . 1.510(4) yes
C12 C17 . 1.511(4) yes
C13 C14 . 1.535(4) yes
C14 C15 . 1.512(5) yes
C15 C16 . 1.513(5) yes
C16 C17 . 1.519(4) yes
