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#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/10/4001068.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_4001068
loop_
_publ_author_name
'Mandal, Trinanjana'
'Stavila, Vitalie'
'Rusakova, Irene'
'Ghosh, Saunab'
'Whitmire, Kenton H.'
_publ_section_title
;
 Molecular Precursors for CdS Nanoparticles: Synthesis and
 Characterization of Carboxylate−Thiourea or
 −Thiosemicarbazide Cadmium Complexes and Their Decomposition
;
_journal_issue                   23
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5617
_journal_paper_doi               10.1021/cm902230u
_journal_volume                  21
_journal_year                    2009
_chemical_formula_sum            'C14 H22 Cd N8 O6 S2'
_chemical_formula_weight         574.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 111.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.039(4)
_cell_length_b                   8.9330(18)
_cell_length_c                   13.876(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2197.7(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.901
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.1657
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22554
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.595
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4913
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.595
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0296
_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)+(0.0161P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                2166
_reflns_number_total             4913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm902230u_si_002.cif
_cod_data_source_block           Compound2b
_cod_original_cell_volume        2197.8(8)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4001068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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 0.0000 0.22660(5) 0.2500 0.03359(13) Uani 1 2 d S
Cd2 Cd 0.5000 0.27169(5) 0.2500 0.03412(13) Uani 1 2 d S
S1 S 0.10172(6) 0.44693(11) 0.28540(9) 0.0408(3) Uani 1 1 d .
S2 S 0.39934(6) 0.49156(15) 0.17144(9) 0.0423(3) Uani 1 1 d .
N1 N 0.0160(2) 0.1981(4) 0.4242(3) 0.0342(9) Uani 1 1 d .
N2 N 0.4900(2) 0.2215(4) 0.4103(3) 0.0377(9) Uani 1 1 d .
N31 N 0.2056(2) 0.2357(4) 0.3078(3) 0.0459(10) Uani 1 1 d .
H31A H 0.2513 0.2061 0.3219 0.055 Uiso 1 1 calc R
H31B H 0.1693 0.1718 0.2899 0.055 Uiso 1 1 calc R
N32 N 0.24797(16) 0.4747(4) 0.3414(2) 0.0392(8) Uani 1 1 d .
H32A H 0.2394 0.5692 0.3408 0.047 Uiso 1 1 calc R
N33 N 0.32154(17) 0.4215(4) 0.3715(3) 0.0500(10) Uani 1 1 d .
H33A H 0.3299 0.3269 0.3719 0.060 Uiso 1 1 calc R
H33B H 0.3587 0.4834 0.3896 0.060 Uiso 1 1 calc R
N41 N 0.2851(2) 0.2949(4) 0.1097(3) 0.0487(10) Uani 1 1 d .
H41A H 0.2379 0.2728 0.0847 0.058 Uiso 1 1 calc R
H41B H 0.3183 0.2248 0.1263 0.058 Uiso 1 1 calc R
N42 N 0.25507(17) 0.5423(4) 0.0967(2) 0.0428(9) Uani 1 1 d .
H42A H 0.2687 0.6346 0.1017 0.051 Uiso 1 1 calc R
N43 N 0.17817(16) 0.5055(4) 0.0611(3) 0.0554(10) Uani 1 1 d .
H43A H 0.1645 0.4132 0.0561 0.067 Uiso 1 1 calc R
H43B H 0.1447 0.5753 0.0444 0.067 Uiso 1 1 calc R
O11 O 0.09036(14) 0.0437(3) 0.3243(2) 0.0362(7) Uani 1 1 d .
O12 O 0.16835(14) -0.0534(3) 0.47123(19) 0.0437(8) Uani 1 1 d .
O21 O 0.40548(15) 0.0976(3) 0.2274(2) 0.0379(7) Uani 1 1 d .
O22 O 0.32566(15) 0.0019(4) 0.2937(2) 0.0542(8) Uani 1 1 d .
C11 C 0.1141(2) 0.0265(4) 0.4217(3) 0.0315(9) Uani 1 1 d .
C12 C 0.0735(2) 0.1115(4) 0.4803(3) 0.0307(9) Uani 1 1 d .
C13 C 0.0951(2) 0.1018(4) 0.5862(3) 0.0357(10) Uani 1 1 d .
H13A H 0.1356 0.0413 0.6238 0.043 Uiso 1 1 calc R
C14 C 0.0569(3) 0.1814(5) 0.6363(3) 0.0466(12) Uani 1 1 d .
H14A H 0.0712 0.1756 0.7078 0.056 Uiso 1 1 calc R
C15 C -0.0038(3) 0.2711(5) 0.5781(4) 0.0446(14) Uani 1 1 d .
H15A H -0.0313 0.3256 0.6094 0.054 Uiso 1 1 calc R
C16 C -0.0214(3) 0.2760(4) 0.4726(4) 0.0426(11) Uani 1 1 d .
H16A H -0.0613 0.3363 0.4330 0.051 Uiso 1 1 calc R
C21 C 0.3836(2) 0.0721(4) 0.3015(3) 0.0350(10) Uani 1 1 d .
C22 C 0.4314(2) 0.1319(4) 0.4064(3) 0.0310(9) Uani 1 1 d .
C23 C 0.4154(2) 0.1019(4) 0.4935(3) 0.0387(11) Uani 1 1 d .
H23A H 0.3743 0.0419 0.4887 0.046 Uiso 1 1 calc R
C24 C 0.4591(3) 0.1591(5) 0.5862(4) 0.0518(13) Uani 1 1 d .
H24A H 0.4479 0.1396 0.6448 0.062 Uiso 1 1 calc R
C25 C 0.5214(4) 0.2480(5) 0.5932(4) 0.0500(15) Uani 1 1 d .
H25A H 0.5537 0.2862 0.6562 0.060 Uiso 1 1 calc R
C26 C 0.5325(3) 0.2761(5) 0.5018(4) 0.0508(13) Uani 1 1 d .
H26A H 0.5726 0.3377 0.5048 0.061 Uiso 1 1 calc R
C31 C 0.1914(2) 0.3781(4) 0.3137(3) 0.0329(10) Uani 1 1 d .
C41 C 0.3064(2) 0.4360(4) 0.1224(3) 0.0346(10) Uani 1 1 d .
O1 O 0.28008(19) -0.1504(3) 0.1003(3) 0.0591(10) Uani 1 1 d D
H1A H 0.298(2) -0.103(4) 0.1545(19) 0.089 Uiso 1 1 d D
H1B H 0.2459(19) -0.098(4) 0.063(3) 0.089 Uiso 1 1 d D
O2 O 0.2434(3) 0.7858(3) 0.3585(4) 0.0746(12) Uani 1 1 d D
H2A H 0.260(3) 0.848(4) 0.330(4) 0.112 Uiso 1 1 d D
H2B H 0.215(3) 0.831(5) 0.381(4) 0.112 Uiso 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'
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
O11 Cd1 O11 90.64(12) 2 .
O11 Cd1 N1 100.30(11) 2 .
O11 Cd1 N1 70.60(11) . .
O11 Cd1 N1 70.60(11) 2 2
O11 Cd1 N1 100.30(11) . 2
N1 Cd1 N1 167.47(16) . 2
O11 Cd1 S1 165.26(7) 2 .
O11 Cd1 S1 93.81(7) . .
N1 Cd1 S1 94.44(9) . .
N1 Cd1 S1 94.76(9) 2 .
O11 Cd1 S1 93.81(7) 2 2
O11 Cd1 S1 165.26(7) . 2
N1 Cd1 S1 94.76(9) . 2
N1 Cd1 S1 94.44(9) 2 2
S1 Cd1 S1 85.40(5) . 2
O21 Cd2 O21 95.44(13) 2_655 .
O21 Cd2 N2 94.08(11) 2_655 .
O21 Cd2 N2 70.83(12) . .
O21 Cd2 N2 70.83(12) 2_655 2_655
O21 Cd2 N2 94.08(11) . 2_655
N2 Cd2 N2 157.95(16) . 2_655
O21 Cd2 S2 91.83(7) 2_655 2_655
O21 Cd2 S2 162.39(7) . 2_655
N2 Cd2 S2 92.71(10) . 2_655
N2 Cd2 S2 103.46(10) 2_655 2_655
O21 Cd2 S2 162.39(7) 2_655 .
O21 Cd2 S2 91.83(7) . .
N2 Cd2 S2 103.46(10) . .
N2 Cd2 S2 92.71(10) 2_655 .
S2 Cd2 S2 85.86(5) 2_655 .
C31 S1 Cd1 111.73(14) . .
C41 S2 Cd2 115.39(15) . .
C12 N1 C16 118.8(4) . .
C12 N1 Cd1 115.9(3) . .
C16 N1 Cd1 124.7(3) . .
C26 N2 C22 117.4(4) . .
C26 N2 Cd2 127.4(3) . .
C22 N2 Cd2 115.1(3) . .
C31 N32 N33 119.3(3) . .
C41 N42 N43 120.2(3) . .
C11 O11 Cd1 118.5(2) . .
C21 O21 Cd2 118.8(3) . .
O12 C11 O11 124.2(4) . .
O12 C11 C12 118.5(3) . .
O11 C11 C12 117.3(3) . .
N1 C12 C13 121.5(4) . .
N1 C12 C11 116.6(4) . .
C13 C12 C11 121.9(4) . .
C14 C13 C12 120.0(4) . .
C13 C14 C15 118.9(4) . .
C16 C15 C14 117.5(5) . .
N1 C16 C15 123.3(4) . .
O22 C21 O21 124.5(4) . .
O22 C21 C22 118.1(4) . .
O21 C21 C22 117.4(4) . .
N2 C22 C23 121.4(4) . .
N2 C22 C21 116.5(3) . .
C23 C22 C21 122.1(4) . .
C24 C23 C22 120.4(4) . .
C23 C24 C25 119.5(4) . .
C26 C25 C24 116.5(5) . .
N2 C26 C25 124.7(5) . .
N31 C31 N32 119.1(4) . .
N31 C31 S1 123.0(3) . .
N32 C31 S1 117.9(3) . .
N42 C41 N41 119.5(4) . .
N42 C41 S2 117.0(3) . .
N41 C41 S2 123.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O11 2.324(3) 2
Cd1 O11 2.324(3) .
Cd1 N1 2.337(4) .
Cd1 N1 2.337(4) 2
Cd1 S1 2.6782(12) .
Cd1 S1 2.6782(12) 2
Cd2 O21 2.312(3) 2_655
Cd2 O21 2.312(3) .
Cd2 N2 2.344(4) .
Cd2 N2 2.344(4) 2_655
Cd2 S2 2.6826(13) 2_655
Cd2 S2 2.6826(13) .
S1 C31 1.720(4) .
S2 C41 1.721(4) .
N1 C12 1.334(5) .
N1 C16 1.339(6) .
N2 C26 1.325(6) .
N2 C22 1.359(5) .
N31 C31 1.309(4) .
N32 C31 1.324(4) .
N32 N33 1.391(4) .
N41 C41 1.316(5) .
N42 C41 1.315(4) .
N42 N43 1.403(4) .
O11 C11 1.268(4) .
O12 C11 1.238(4) .
O21 C21 1.263(4) .
O22 C21 1.239(4) .
C11 C12 1.514(5) .
C12 C13 1.377(5) .
C13 C14 1.374(5) .
C14 C15 1.397(6) .
C15 C16 1.379(7) .
C21 C22 1.505(5) .
C22 C23 1.377(5) .
C23 C24 1.351(5) .
C24 C25 1.402(7) .
C25 C26 1.382(7) .
