#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:32:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179900 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/96/7019602.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_7019602
loop_
_publ_author_name
'Dey, Sandeep Kumar'
'Das, Gopal'
_publ_section_title
;
 Selective inclusion of PO(4)(3-) within persistent dimeric capsules of a
 tris(thiourea) receptor and evidence of cation/solvent sealed
 unimolecular capsules.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8960
_journal_page_last               8972
_journal_paper_doi               10.1039/c2dt30687e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         '2(C27 H30 N10 O6 S3), 2(C8 H20 N), C O3'
_chemical_formula_sum            'C71 H100 N22 O15 S6'
_chemical_formula_weight         1694.15
_chemical_name_systematic
;
?
;
_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                 108.323(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2809(7)
_cell_length_b                   19.0630(7)
_cell_length_c                   24.6347(9)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.13
_cell_measurement_theta_min      2.23
_cell_volume                     8595.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Mercury 2.3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61244
_diffrn_reflns_theta_full        24.78
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7338
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.3000P)²+0.3500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2487
_reflns_number_gt                3976
_reflns_number_total             7338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30687e.txt
_cod_data_source_block           Carbonate
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7019602
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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C13 C -0.21972(16) 0.25504(19) 0.28275(14) 0.0796(13) Uani 1 1 d G
C14 C -0.2740(2) 0.29335(19) 0.29538(17) 0.0993(16) Uani 1 1 d G
H14 H -0.2618 0.3248 0.3258 0.119 Uiso 1 1 calc R
C15 C -0.3467(2) 0.2847(2) 0.2625(2) 0.123(2) Uani 1 1 d G
H15 H -0.3831 0.3104 0.2710 0.148 Uiso 1 1 calc R
C16 C -0.36505(16) 0.2378(3) 0.2171(2) 0.123(2) Uani 1 1 d G
C17 C -0.3107(2) 0.1994(2) 0.20443(18) 0.127(2) Uani 1 1 d G
H17 H -0.3230 0.1680 0.1740 0.152 Uiso 1 1 calc R
C18 C -0.23807(19) 0.2081(2) 0.23728(17) 0.1057(18) Uani 1 1 d G
H18 H -0.2017 0.1824 0.2288 0.127 Uiso 1 1 calc R
C22 C 0.0806(2) 0.0300(2) 0.20996(12) 0.0814(14) Uani 1 1 d G
C23 C 0.0847(2) 0.06647(19) 0.16223(16) 0.110(2) Uani 1 1 d G
H23 H 0.0952 0.1142 0.1648 0.132 Uiso 1 1 calc R
C24 C 0.0733(3) 0.0316(3) 0.11060(12) 0.131(3) Uani 1 1 d G
H24 H 0.0761 0.0560 0.0787 0.158 Uiso 1 1 calc R
C25 C 0.0577(3) -0.0398(3) 0.10671(16) 0.137(3) Uani 1 1 d G
C26 C 0.0535(3) -0.0762(2) 0.1544(2) 0.164(4) Uani 1 1 d G
H26 H 0.0430 -0.1240 0.1518 0.197 Uiso 1 1 calc R
C27 C 0.0649(3) -0.0413(2) 0.20607(18) 0.1110(19) Uani 1 1 d G
H27 H 0.0621 -0.0658 0.2380 0.133 Uiso 1 1 calc R
N1 N 0.1144(2) 0.2287(2) 0.41476(17) 0.0858(12) Uani 1 1 d .
C4 C 0.1218(3) 0.4366(2) 0.2182(2) 0.0851(14) Uani 1 1 d .
C3 C 0.1787(3) 0.3797(3) 0.3136(2) 0.0836(14) Uani 1 1 d .
C5 C 0.1821(3) 0.4698(3) 0.2093(3) 0.1011(17) Uani 1 1 d .
H5 H 0.2286 0.4622 0.2347 0.121 Uiso 1 1 calc R
C7 C 0.1071(5) 0.5226(4) 0.1248(3) 0.117(2) Uani 1 1 d .
C9 C 0.0545(4) 0.4456(4) 0.1774(3) 0.1095(18) Uani 1 1 d .
H9 H 0.0141 0.4223 0.1814 0.131 Uiso 1 1 calc R
C2 C 0.2130(3) 0.3019(4) 0.3972(3) 0.121(2) Uani 1 1 d .
H2A H 0.2626 0.2988 0.3958 0.145 Uiso 1 1 calc R
H2B H 0.2121 0.3371 0.4254 0.145 Uiso 1 1 calc R
C1 C 0.1922(4) 0.2348(6) 0.4149(3) 0.156(3) Uani 1 1 d .
H1A H 0.2241 0.2250 0.4533 0.187 Uiso 1 1 calc R
H1B H 0.2008 0.1989 0.3899 0.187 Uiso 1 1 calc R
C6 C 0.1733(4) 0.5126(3) 0.1640(3) 0.113(2) Uani 1 1 d .
H6 H 0.2137 0.5357 0.1596 0.135 Uiso 1 1 calc R
C8 C 0.0461(5) 0.4887(4) 0.1307(4) 0.138(3) Uani 1 1 d .
H8 H 0.0004 0.4948 0.1036 0.166 Uiso 1 1 calc R
N3 N 0.1245(2) 0.3923(2) 0.26227(17) 0.0799(11) Uani 1 1 d .
H3 H 0.0856 0.3677 0.2573 0.096 Uiso 1 1 calc R
N2 N 0.1652(2) 0.3243(3) 0.34147(18) 0.1002(14) Uani 1 1 d .
H2 H 0.1262 0.3004 0.3258 0.120 Uiso 1 1 calc R
N4 N 0.0964(7) 0.5710(4) 0.0777(4) 0.161(3) Uani 1 1 d .
S1 S 0.25499(10) 0.42647(11) 0.34026(8) 0.1226(7) Uani 1 1 d .
O2 O 0.1509(5) 0.6050(4) 0.0761(3) 0.177(3) Uani 1 1 d .
O1 O 0.0350(6) 0.5735(4) 0.0401(3) 0.210(4) Uani 1 1 d .
C12 C -0.1102(3) 0.2740(3) 0.3691(2) 0.0864(15) Uani 1 1 d .
C11 C 0.0131(4) 0.2839(5) 0.4408(3) 0.125(3) Uani 1 1 d .
H11A H 0.0043 0.2470 0.4649 0.150 Uiso 1 1 calc R
H11B H 0.0036 0.3284 0.4562 0.150 Uiso 1 1 calc R
C10 C 0.0918(6) 0.2817(6) 0.4434(3) 0.170(4) Uani 1 1 d .
H10A H 0.1032 0.3260 0.4288 0.204 Uiso 1 1 calc R
H10B H 0.1211 0.2790 0.4833 0.204 Uiso 1 1 calc R
N6 N -0.1465(2) 0.2601(2) 0.31263(16) 0.0823(11) Uani 1 1 d .
H6A H -0.1182 0.2534 0.2922 0.099 Uiso 1 1 calc R
N5 N -0.0380(3) 0.2757(2) 0.38310(16) 0.0911(13) Uani 1 1 d .
H5A H -0.0196 0.2716 0.3557 0.109 Uiso 1 1 calc R
N7 N -0.4396(4) 0.2247(5) 0.1836(4) 0.171(3) Uani 1 1 d D
S2 S -0.15298(12) 0.28461(17) 0.41786(8) 0.1564(10) Uani 1 1 d .
O3 O -0.4863(4) 0.2638(5) 0.1934(4) 0.215(4) Uani 1 1 d D
O4 O -0.4534(4) 0.1782(6) 0.1460(5) 0.261(5) Uani 1 1 d D
C21 C 0.1086(2) 0.0520(3) 0.3144(2) 0.0749(12) Uani 1 1 d .
C20 C 0.1216(4) 0.0986(3) 0.4090(2) 0.1073(19) Uani 1 1 d .
H20A H 0.0954 0.0606 0.4201 0.129 Uiso 1 1 calc R
H20B H 0.1733 0.0876 0.4232 0.129 Uiso 1 1 calc R
C19 C 0.1092(6) 0.1608(4) 0.4354(3) 0.153(3) Uani 1 1 d .
H19A H 0.0603 0.1569 0.4382 0.184 Uiso 1 1 calc R
H19B H 0.1424 0.1595 0.4742 0.184 Uiso 1 1 calc R
N9 N 0.0877(2) 0.0699(2) 0.25822(15) 0.0755(10) Uani 1 1 d .
H9A H 0.0771 0.1135 0.2516 0.091 Uiso 1 1 calc R
N8 N 0.0993(2) 0.1024(2) 0.34725(15) 0.0839(12) Uani 1 1 d .
H8A H 0.0784 0.1403 0.3312 0.101 Uiso 1 1 calc R
S3 S 0.14490(10) -0.02658(9) 0.34100(7) 0.1111(7) Uani 1 1 d .
N11 N 0.1863(4) 0.6082(3) 0.4291(3) 0.1176(17) Uani 1 1 d .
C30 C 0.1275(5) 0.6568(5) 0.4332(4) 0.145(3) Uani 1 1 d D
H30A H 0.1248 0.6543 0.4718 0.174 Uiso 1 1 calc R
H30B H 0.0813 0.6398 0.4077 0.174 Uiso 1 1 calc R
C28 C 0.1702(9) 0.5380(8) 0.4384(4) 0.221(6) Uani 1 1 d D
H28A H 0.2054 0.5088 0.4282 0.265 Uiso 1 1 calc R
H28B H 0.1227 0.5274 0.4113 0.265 Uiso 1 1 calc R
C32 C 0.1933(7) 0.6134(6) 0.3681(5) 0.178(4) Uani 1 1 d D
H32A H 0.2093 0.6602 0.3625 0.214 Uiso 1 1 calc R
H32B H 0.2303 0.5806 0.3650 0.214 Uiso 1 1 calc R
C29 C 0.1688(11) 0.5144(10) 0.4965(5) 0.276(8) Uani 1 1 d D
H29A H 0.2013 0.5432 0.5255 0.414 Uiso 1 1 calc R
H29B H 0.1841 0.4664 0.5025 0.414 Uiso 1 1 calc R
H29C H 0.1200 0.5187 0.4985 0.414 Uiso 1 1 calc R
C31 C 0.1354(5) 0.7329(5) 0.4192(4) 0.166(3) Uani 1 1 d D
H31A H 0.1789 0.7518 0.4460 0.249 Uiso 1 1 calc R
H31B H 0.0937 0.7587 0.4214 0.249 Uiso 1 1 calc R
H31C H 0.1387 0.7365 0.3812 0.249 Uiso 1 1 calc R
C33 C 0.1225(8) 0.5977(7) 0.3217(5) 0.269(9) Uani 1 1 d D
H33A H 0.1073 0.5507 0.3262 0.404 Uiso 1 1 calc R
H33B H 0.1295 0.6024 0.2850 0.404 Uiso 1 1 calc R
H33C H 0.0856 0.6301 0.3244 0.404 Uiso 1 1 calc R
C34 C 1.0000 0.2447(4) 0.2500 0.0653(15) Uani 1 2 d S
O8 O 0.9442(2) 0.2136(2) 0.2515(2) 0.1079(13) Uani 1 1 d .
O7 O 1.0000 0.3105(3) 0.2500 0.165(4) Uani 1 2 d S
C35 C 0.2557(6) 0.6308(7) 0.4728(6) 0.189(4) Uani 1 1 d D
H35A H 0.2471 0.6303 0.5096 0.227 Uiso 1 1 calc R
H35B H 0.2638 0.6794 0.4647 0.227 Uiso 1 1 calc R
C36 C 0.3264(8) 0.5921(9) 0.4804(11) 0.321(12) Uani 1 1 d D
H36A H 0.3271 0.5498 0.5016 0.482 Uiso 1 1 calc R
H36B H 0.3668 0.6214 0.5007 0.482 Uiso 1 1 calc R
H36C H 0.3304 0.5806 0.4435 0.482 Uiso 1 1 calc R
N10 N 0.0470(5) -0.0766(5) 0.0530(4) 0.203(5) Uani 1 1 d DU
O6 O 0.0685(6) -0.0461(5) 0.0164(3) 0.246(5) Uani 1 1 d DU
O5 O 0.0246(6) -0.1384(6) 0.0508(4) 0.322(9) Uani 1 1 d D
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'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
N6 C13 C14 124.2(3) .
N6 C13 C18 115.8(3) .
C14 C13 C18 120.0 .
C15 C14 C13 120.0 .
C14 C15 C16 120.0 .
C17 C16 C15 120.0 .
C17 C16 N7 118.0(5) .
C15 C16 N7 122.0(5) .
C18 C17 C16 120.0 .
C17 C18 C13 120.0 .
N9 C22 C23 115.9(3) .
N9 C22 C27 124.0(3) .
C23 C22 C27 120.0 .
C22 C23 C24 120.0 .
C25 C24 C23 120.0 .
C26 C25 C24 120.0 .
C26 C25 N10 119.9(6) .
C24 C25 N10 120.1(6) .
C25 C26 C27 120.0 .
C26 C27 C22 120.0 .
C10 N1 C19 114.8(7) .
C10 N1 C1 114.7(7) .
C19 N1 C1 104.8(7) .
N3 C4 C9 116.7(5) .
N3 C4 C5 125.3(5) .
C9 C4 C5 117.8(5) .
N2 C3 N3 113.3(4) .
N2 C3 S1 120.8(4) .
N3 C3 S1 125.9(4) .
C6 C5 C4 120.5(6) .
C6 C7 C8 120.1(6) .
C6 C7 N4 121.9(9) .
C8 C7 N4 117.9(9) .
C4 C9 C8 121.3(7) .
C1 C2 N2 112.9(5) .
C2 C1 N1 116.0(8) .
C7 C6 C5 121.5(7) .
C9 C8 C7 118.7(7) .
C4 N3 C3 131.6(4) .
C3 N2 C2 123.4(5) .
O2 N4 O1 124.4(8) .
O2 N4 C7 116.7(11) .
O1 N4 C7 118.8(10) .
N5 C12 N6 115.2(4) .
N5 C12 S2 121.8(4) .
N6 C12 S2 122.9(4) .
N5 C11 C10 113.8(5) .
N1 C10 C11 118.5(8) .
C12 N6 C13 131.7(4) .
C12 N5 C11 126.0(4) .
O4 N7 O3 124.7(10) .
O4 N7 C16 119.3(7) .
O3 N7 C16 115.9(8) .
N8 C21 N9 113.1(4) .
N8 C21 S3 122.1(4) .
N9 C21 S3 124.8(4) .
C19 C20 N8 113.9(5) .
N1 C19 C20 124.6(6) .
C21 N9 C22 131.0(4) .
C21 N8 C20 124.2(5) .
C28 N11 C30 111.6(8) .
C28 N11 C35 110.6(9) .
C30 N11 C35 107.4(7) .
C28 N11 C32 107.9(7) .
C30 N11 C32 108.9(7) .
C35 N11 C32 110.4(8) .
N11 C30 C31 116.6(7) .
N11 C28 C29 120.5(12) .
C33 C32 N11 112.8(8) .
O8 C34 O8 122.9(7) 2_755
O8 C34 O7 118.5(3) 2_755
O8 C34 O7 118.5(3) .
N11 C35 C36 121.2(13) .
O5 N10 O6 126.5(9) .
O5 N10 C25 116.3(8) .
O6 N10 C25 116.6(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C13 N6 1.376(5) .
C13 C14 1.3900 .
C13 C18 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
C16 C17 1.3900 .
C16 N7 1.437(9) .
C17 C18 1.3900 .
C22 N9 1.381(4) .
C22 C23 1.3900 .
C22 C27 1.3900 .
C23 C24 1.3900 .
C24 C25 1.3900 .
C25 C26 1.3900 .
C25 N10 1.453(9) .
C26 C27 1.3900 .
N1 C10 1.379(9) .
N1 C19 1.406(8) .
N1 C1 1.503(9) .
C4 N3 1.364(6) .
C4 C9 1.380(8) .
C4 C5 1.400(8) .
C3 N2 1.329(6) .
C3 N3 1.384(6) .
C3 S1 1.668(5) .
C5 C6 1.349(8) .
C7 C6 1.349(10) .
C7 C8 1.389(11) .
C7 N4 1.446(10) .
C9 C8 1.381(10) .
C2 C1 1.449(12) .
C2 N2 1.455(7) .
N4 O2 1.247(11) .
N4 O1 1.254(13) .
C12 N5 1.326(7) .
C12 N6 1.373(6) .
C12 S2 1.668(5) .
C11 N5 1.461(8) .
C11 C10 1.499(13) .
N7 O4 1.2494(10) .
N7 O3 1.2494(10) .
C21 N8 1.306(6) .
C21 N9 1.357(6) .
C21 S3 1.695(5) .
C20 C19 1.407(9) .
C20 N8 1.448(6) .
N11 C28 1.408(14) .
N11 C30 1.492(10) .
N11 C35 1.493(12) .
N11 C32 1.553(11) .
C30 C31 1.5100(10) .
C28 C29 1.5094(10) .
C32 C33 1.5099(10) .
C34 O8 1.238(4) 2_755
C34 O8 1.238(4) .
C34 O7 1.254(8) .
C35 C36 1.5099(10) .
N10 O5 1.2496(10) .
N10 O6 1.2496(10) .
