#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:58:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179945 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/40/7024050.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_7024050
loop_
_publ_author_name
'Paul, Avijit Kumar'
'Madras, Giridhar'
'Natarajan, Srinivasan'
_publ_section_title
;
 Synthesis, structure, transformation studies and catalytic properties of
 open-framework cadmium thiosulfate compounds.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2263
_journal_page_last               2279
_journal_paper_doi               10.1039/b908995k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C60 H68 Cd2 N12 O20 S8'
_chemical_formula_weight         1758.42
_chemical_name_common            '1D-Cadmium thiosulfate'
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.228(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.420(3)
_cell_length_b                   17.361(4)
_cell_length_c                   15.840(3)
_cell_measurement_reflns_used    8352
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      1.96
_cell_volume                     3560.9(13)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        Saint
_computing_molecular_graphics
'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al.,1993)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'φ and ω 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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37720
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.9225
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Block like'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.522
_refine_diff_density_min         -2.159
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0661P)²+15.5599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                5371
_reflns_number_total             8352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908995k.txt
_cod_data_source_block           Compound(2)
_cod_original_cell_volume        3560.8(12)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7024050
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
Cd1 Cd 0.7500 0.72100(3) 0.2500 0.03254(16) Uani 1 2 d S
Cd2 Cd 0.2500 0.22024(3) 0.2500 0.03365(16) Uani 1 2 d S
S1 S 0.65816(14) 0.76471(11) 0.35834(10) 0.0582(5) Uani 1 1 d .
S2 S 0.34938(15) 0.26632(11) 0.14720(11) 0.0596(5) Uani 1 1 d .
S3 S 0.55243(15) 0.82366(13) 0.26584(11) 0.0647(6) Uani 1 1 d .
S4 S 0.4690(3) 0.2993(2) 0.24836(15) 0.1175(13) Uani 1 1 d .
N1 N 0.6556(4) 0.6284(3) 0.1523(3) 0.0412(11) Uani 1 1 d .
N2 N 0.1556(4) 0.1290(3) 0.1531(3) 0.0379(10) Uani 1 1 d .
O1 O 0.5615(5) 0.7956(4) 0.1826(3) 0.0826(17) Uani 1 1 d .
O6 O 0.4250(5) 0.3064(4) 0.3235(3) 0.0891(19) Uani 1 1 d .
N5 N 0.3802(4) 0.7403(3) 0.9592(5) 0.0605(15) Uani 1 1 d .
N4 N 0.5026(4) 0.8648(3) 0.9520(4) 0.0570(14) Uani 1 1 d .
H4B H 0.4615 0.8266 0.9512 0.068 Uiso 1 1 calc R
C3 C 0.5331(4) 0.5263(3) 0.0321(3) 0.0328(11) Uani 1 1 d .
C2 C 0.5771(5) 0.5917(3) 0.0060(4) 0.0459(14) Uani 1 1 d .
H2 H 0.5657 0.6027 -0.0532 0.055 Uiso 1 1 calc R
C13 C 0.7033(4) 1.0539(3) 0.9602(4) 0.0430(13) Uani 1 1 d .
C25 C 0.2558(4) 0.6125(3) 0.9663(4) 0.0427(13) Uani 1 1 d .
C16 C 0.6333(4) 0.9868(3) 0.9562(4) 0.0425(13) Uani 1 1 d .
C9C C 0.0534(5) 0.0152(4) 0.1217(4) 0.0499(16) Uani 1 1 d .
H9 H 0.0267 -0.0277 0.1434 0.060 Uiso 1 1 calc R
C7 C 0.0767(5) 0.0915(3) 0.0058(4) 0.0434(14) Uani 1 1 d .
H7 H 0.0661 0.1021 -0.0535 0.052 Uiso 1 1 calc R
C8 C 0.0328(4) 0.0273(3) 0.0324(3) 0.0334(11) Uani 1 1 d .
C4 C 0.5524(6) 0.5145(4) 0.1208(4) 0.0600(19) Uani 1 1 d .
H4 H 0.5254 0.4717 0.1422 0.072 Uiso 1 1 calc R
O3 O 0.4547(4) 0.8114(6) 0.2817(5) 0.124(3) Uani 1 1 d .
C6 C 0.1362(5) 0.1398(4) 0.0673(4) 0.0476(15) Uani 1 1 d .
H6 H 0.1647 0.1829 0.0477 0.057 Uiso 1 1 calc R
N3 N 0.8345(5) 1.1786(3) 0.9674(5) 0.0652(16) Uani 1 1 d .
O5 O 0.5182(6) 0.3615(4) 0.2268(4) 0.102(2) Uani 1 1 d .
C17 C 0.5399(5) 0.9811(4) 0.8921(4) 0.0514(15) Uani 1 1 d .
H17 H 0.5202 1.0192 0.8498 0.062 Uiso 1 1 calc R
N6 N 0.0752(6) 0.4136(3) 0.9728(5) 0.0681(17) Uani 1 1 d .
C27 C 0.2153(6) 0.4939(4) 1.0392(5) 0.0621(19) Uani 1 1 d .
H27 H 0.2716 0.5038 1.0865 0.074 Uiso 1 1 calc R
O2 O 0.5800(7) 0.9070(3) 0.2766(4) 0.117(3) Uani 1 1 d .
C20 C 0.6592(5) 0.9287(3) 1.0190(4) 0.0470(14) Uani 1 1 d .
H20 H 0.7209 0.9308 1.0627 0.056 Uiso 1 1 calc R
C26 C 0.1916(5) 0.5436(3) 0.9687(4) 0.0436(13) Uani 1 1 d .
C10 C 0.1134(5) 0.0668(4) 0.1777(4) 0.0531(17) Uani 1 1 d .
H10 H 0.1255 0.0577 0.2374 0.064 Uiso 1 1 calc R
C15 C 0.8306(5) 1.1410(4) 1.0403(5) 0.0599(18) Uani 1 1 d .
H15 H 0.8724 1.1578 1.0936 0.072 Uiso 1 1 calc R
C19 C 0.5923(5) 0.8689(4) 1.0149(5) 0.0554(17) Uani 1 1 d .
H19 H 0.6089 0.8299 1.0565 0.066 Uiso 1 1 calc R
C1 C 0.6371(5) 0.6400(3) 0.0671(4) 0.0447(14) Uani 1 1 d .
H1 H 0.6660 0.6830 0.0477 0.054 Uiso 1 1 calc R
C30 C 0.1071(5) 0.5265(4) 0.9005(5) 0.0573(17) Uani 1 1 d .
H30 H 0.0886 0.5586 0.8519 0.069 Uiso 1 1 calc R
C22 C 0.3136(5) 0.6485(4) 1.0414(5) 0.0542(16) Uani 1 1 d .
H22 H 0.3110 0.6303 1.0960 0.065 Uiso 1 1 calc R
C5 C 0.6127(6) 0.5673(4) 0.1780(4) 0.063(2) Uani 1 1 d .
H5 H 0.6234 0.5591 0.2378 0.075 Uiso 1 1 calc R
C12 C 0.7071(5) 1.0934(4) 0.8859(5) 0.0558(16) Uani 1 1 d .
H12 H 0.6648 1.0786 0.8319 0.067 Uiso 1 1 calc R
C23 C 0.2622(6) 0.6445(4) 0.8876(5) 0.0593(18) Uani 1 1 d .
H23 H 0.2242 0.6235 0.8349 0.071 Uiso 1 1 calc R
C29 C 0.0506(6) 0.4616(4) 0.9051(5) 0.0659(19) Uani 1 1 d .
H29 H -0.0069 0.4507 0.8592 0.079 Uiso 1 1 calc R
C11 C 0.7737(6) 1.1551(4) 0.8912(5) 0.067(2) Uani 1 1 d .
H11 H 0.7761 1.1808 0.8403 0.080 Uiso 1 1 calc R
C24 C 0.3244(6) 0.7068(4) 0.8878(5) 0.067(2) Uani 1 1 d .
H24 H 0.3276 0.7268 0.8341 0.080 Uiso 1 1 calc R
C28 C 0.1551(8) 0.4295(5) 1.0393(6) 0.079(2) Uani 1 1 d .
H28 H 0.1711 0.3966 1.0873 0.095 Uiso 1 1 calc R
C21 C 0.3745(5) 0.7106(4) 1.0357(5) 0.0615(19) Uani 1 1 d .
H21 H 0.4134 0.7330 1.0871 0.074 Uiso 1 1 calc R
C18 C 0.4774(5) 0.9184(4) 0.8921(5) 0.0593(17) Uani 1 1 d .
H18 H 0.4159 0.9140 0.8485 0.071 Uiso 1 1 calc R
C14 C 0.7676(5) 1.0789(4) 1.0393(5) 0.0534(16) Uani 1 1 d .
H14 H 0.7678 1.0536 1.0911 0.064 Uiso 1 1 calc R
O4 O 0.5541(7) 0.2311(6) 0.2641(8) 0.181(5) Uani 1 1 d .
H4A H 0.5718 0.2237 0.2190 0.271 Uiso 1 1 calc R
O100 O -0.0355(5) 0.3013(3) 1.0085(4) 0.0918(19) Uani 1 1 d .
O300 O 0.7500 0.9840(5) 0.2500 0.121(4) Uani 1 2 d S
O200 O 0.2500 0.8583(8) 0.7500 0.175(6) Uani 1 2 d S
O400 O 0.8585(10) 0.3432(6) 0.7768(7) 0.193(5) Uani 1 1 d .
O500 O 0.3562(11) 0.4570(16) 1.2382(7) 0.46(2) Uani 1 1 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'
Cd Cd -0.8075 1.2024 '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
_geom_angle_site_symmetry_3
N1 Cd1 N1 94.0(2) . 2_655
N1 Cd1 S1 112.58(13) . .
N1 Cd1 S1 91.91(12) 2_655 .
N1 Cd1 S1 91.91(12) . 2_655
N1 Cd1 S1 112.58(13) 2_655 2_655
S1 Cd1 S1 144.37(10) . 2_655
N2 Cd2 N2 94.5(2) . 2
N2 Cd2 S2 110.86(12) . 2
N2 Cd2 S2 94.57(12) 2 2
N2 Cd2 S2 94.57(12) . .
N2 Cd2 S2 110.86(12) 2 .
S2 Cd2 S2 142.55(10) 2 .
S3 S1 Cd1 92.01(7) . .
S4 S2 Cd2 91.31(9) . .
O3 S3 O1 114.6(5) . .
O3 S3 O2 109.9(5) . .
O1 S3 O2 110.8(4) . .
O3 S3 S1 107.5(3) . .
O1 S3 S1 106.2(2) . .
O2 S3 S1 107.5(3) . .
O5 S4 O6 117.8(5) . .
O5 S4 O4 104.5(5) . .
O6 S4 O4 110.7(5) . .
O5 S4 S2 111.2(3) . .
O6 S4 S2 105.1(3) . .
O4 S4 S2 107.1(5) . .
C1 N1 C5 117.2(5) . .
C1 N1 Cd1 119.4(4) . .
C5 N1 Cd1 123.2(4) . .
C10 N2 C6 115.6(5) . .
C10 N2 Cd2 124.1(4) . .
C6 N2 Cd2 120.2(4) . .
C24 N5 C21 116.9(6) . .
C18 N4 C19 120.6(6) . .
C18 N4 H4B 119.7 . .
C19 N4 H4B 119.7 . .
C4 C3 C2 116.4(5) . .
C4 C3 C3 122.0(6) . 3_665
C2 C3 C3 121.6(6) . 3_665
C1 C2 C3 120.4(5) . .
C1 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
C12 C13 C14 117.5(6) . .
C12 C13 C16 121.3(6) . .
C14 C13 C16 121.2(6) . .
C22 C25 C23 116.0(6) . .
C22 C25 C26 122.7(6) . .
C23 C25 C26 121.3(6) . .
C17 C16 C20 118.4(6) . .
C17 C16 C13 121.6(6) . .
C20 C16 C13 120.0(6) . .
C10 C9C C8 119.3(5) . .
C10 C9C H9 120.3 . .
C8 C9C H9 120.3 . .
C6 C7 C8 119.5(5) . .
C6 C7 H7 120.2 . .
C8 C7 H7 120.2 . .
C7 C8 C9C 116.7(5) . .
C7 C8 C8 121.6(6) . 3
C9C C8 C8 121.7(6) . 3
C3 C4 C5 119.3(6) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N2 C6 C7 124.2(5) . .
N2 C6 H6 117.9 . .
C7 C6 H6 117.9 . .
C11 N3 C15 118.6(6) . .
C18 C17 C16 119.3(6) . .
C18 C17 H17 120.4 . .
C16 C17 H17 120.4 . .
C28 N6 C29 119.4(7) . .
C28 C27 C26 119.8(8) . .
C28 C27 H27 120.1 . .
C26 C27 H27 120.1 . .
C19 C20 C16 118.6(6) . .
C19 C20 H20 120.7 . .
C16 C20 H20 120.7 . .
C30 C26 C27 117.8(6) . .
C30 C26 C25 121.2(6) . .
C27 C26 C25 121.0(6) . .
N2 C10 C9C 124.7(5) . .
N2 C10 H10 117.7 . .
C9C C10 H10 117.7 . .
N3 C15 C14 122.6(7) . .
N3 C15 H15 118.7 . .
C14 C15 H15 118.7 . .
N4 C19 C20 121.6(6) . .
N4 C19 H19 119.2 . .
C20 C19 H19 119.2 . .
N1 C1 C2 123.0(5) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C29 C30 C26 119.3(7) . .
C29 C30 H30 120.4 . .
C26 C30 H30 120.4 . .
C21 C22 C25 120.5(7) . .
C21 C22 H22 119.8 . .
C25 C22 H22 119.8 . .
N1 C5 C4 123.6(6) . .
N1 C5 H5 118.2 . .
C4 C5 H5 118.2 . .
C13 C12 C11 120.2(7) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C24 C23 C25 119.8(7) . .
C24 C23 H23 120.1 . .
C25 C23 H23 120.1 . .
N6 C29 C30 122.3(7) . .
N6 C29 H29 118.9 . .
C30 C29 H29 118.9 . .
N3 C11 C12 121.7(7) . .
N3 C11 H11 119.2 . .
C12 C11 H11 119.2 . .
N5 C24 C23 124.1(7) . .
N5 C24 H24 118.0 . .
C23 C24 H24 118.0 . .
N6 C28 C27 121.5(8) . .
N6 C28 H28 119.3 . .
C27 C28 H28 119.3 . .
N5 C21 C22 122.7(7) . .
N5 C21 H21 118.6 . .
C22 C21 H21 118.6 . .
N4 C18 C17 121.4(7) . .
N4 C18 H18 119.3 . .
C17 C18 H18 119.3 . .
C15 C14 C13 119.4(7) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
S4 O4 H4A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N1 2.357(4) .
Cd1 N1 2.357(4) 2_655
Cd1 S1 2.4801(16) .
Cd1 S1 2.4801(16) 2_655
Cd2 N2 2.334(4) .
Cd2 N2 2.334(4) 2
Cd2 S2 2.4922(17) 2
Cd2 S2 2.4922(17) .
S1 S3 2.029(2) .
S2 S4 2.030(3) .
S3 O3 1.414(6) .
S3 O1 1.441(5) .
S3 O2 1.491(7) .
S4 O5 1.354(6) .
S4 O6 1.465(6) .
S4 O4 1.619(9) .
N1 C1 1.321(7) .
N1 C5 1.322(7) .
N2 C10 1.324(7) .
N2 C6 1.329(7) .
N5 C24 1.317(10) .
N5 C21 1.338(10) .
N4 C18 1.309(9) .
N4 C19 1.348(9) .
N4 H4B 0.8600 .
C3 C4 1.375(8) .
C3 C2 1.391(7) .
C3 C3 1.478(10) 3_665
C2 C1 1.371(8) .
C2 H2 0.9300 .
C13 C12 1.375(9) .
C13 C14 1.391(9) .
C13 C16 1.488(8) .
C25 C22 1.386(9) .
C25 C23 1.387(9) .
C25 C26 1.481(8) .
C16 C17 1.394(9) .
C16 C20 1.394(8) .
C9C C10 1.364(8) .
C9C C8 1.386(7) .
C9C H9 0.9300 .
C7 C6 1.371(8) .
C7 C8 1.377(7) .
C7 H7 0.9300 .
C8 C8 1.502(10) 3
C4 C5 1.389(9) .
C4 H4 0.9300 .
C6 H6 0.9300 .
N3 C11 1.331(10) .
N3 C15 1.339(9) .
C17 C18 1.373(9) .
C17 H17 0.9300 .
N6 C28 1.320(11) .
N6 C29 1.329(10) .
C27 C28 1.378(11) .
C27 C26 1.381(9) .
C27 H27 0.9300 .
C20 C19 1.364(9) .
C20 H20 0.9300 .
C26 C30 1.378(9) .
C10 H10 0.9300 .
C15 C14 1.368(9) .
C15 H15 0.9300 .
C19 H19 0.9300 .
C1 H1 0.9300 .
C30 C29 1.370(9) .
C30 H30 0.9300 .
C22 C21 1.370(9) .
C22 H22 0.9300 .
C5 H5 0.9300 .
C12 C11 1.383(10) .
C12 H12 0.9300 .
C23 C24 1.367(9) .
C23 H23 0.9300 .
C29 H29 0.9300 .
C11 H11 0.9300 .
C24 H24 0.9300 .
C28 H28 0.9300 .
C21 H21 0.9300 .
C18 H18 0.9300 .
C14 H14 0.9300 .
O4 H4A 0.8200 .
