#------------------------------------------------------------------------------
#$Date: 2016-08-06 09:24:30 +0300 (Sat, 06 Aug 2016) $
#$Revision: 185065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/02/7040206.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_7040206
loop_
_publ_author_name
'Saad, Fawaz A.'
'Knight, James C.'
'Kariuki, Benson M.'
'Amoroso, Angelo J.'
_publ_section_title
;
 Co-ordination behaviour of a novel tristhiourea tripodal ligand;
 structural variations in a series of transition metal complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10280
_journal_page_last               10288
_journal_paper_doi               10.1039/c6dt01148a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C42 H36.5 Cd Cl2 N10 O11.25 S3'
_chemical_formula_weight         1140.79
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.8780(17)
_cell_length_b                   13.8780(17)
_cell_length_c                   43.257(8)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.825
_cell_volume                     7215.1(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1115
_diffrn_reflns_av_unetI/netI     0.2631
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            7891
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             3471
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2976
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1069P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1099
_reflns_number_total             2976
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01148a2.cif
_cod_data_source_block           aja0838
_cod_original_cell_volume        7215(2)
_cod_original_formula_sum        'C42 H36.50 Cd Cl2 N10 O11.25 S3'
_cod_database_code               7040206
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.0726(4) 0.1126(4) 0.27414(16) 0.0452(14) Uani 1 1 d . U .
H1A H 0.1507 0.1310 0.2712 0.054 Uiso 1 1 calc R U .
H1B H 0.0607 0.1159 0.2966 0.054 Uiso 1 1 calc R U .
C2 C 0.0564(5) 0.1988(5) 0.25829(19) 0.0499(15) Uani 1 1 d . U .
C3 C 0.0712(5) 0.2945(5) 0.27278(18) 0.0507(16) Uani 1 1 d . . .
H3 H 0.0831 0.3029 0.2945 0.061 Uiso 1 1 calc R U .
C4 C 0.0689(6) 0.3763(5) 0.2561(2) 0.062(2) Uani 1 1 d . . .
H4 H 0.0826 0.4430 0.2660 0.074 Uiso 1 1 calc R U .
C5 C 0.0464(6) 0.3627(5) 0.22450(18) 0.0524(17) Uani 1 1 d . . .
H5 H 0.0399 0.4174 0.2129 0.063 Uiso 1 1 calc R U .
C6 C 0.0338(4) 0.2673(5) 0.21037(15) 0.0408(13) Uani 1 1 d . . .
C7 C -0.0450(5) 0.1679(5) 0.16089(19) 0.0489(16) Uani 1 1 d . . .
C8 C 0.0142(5) 0.2846(5) 0.11379(18) 0.0462(14) Uani 1 1 d . U .
C9 C -0.0068(5) 0.2834(4) 0.08014(17) 0.0427(14) Uani 1 1 d . U .
C10 C -0.0983(5) 0.1945(6) 0.06603(17) 0.0548(17) Uani 1 1 d . . .
H10 H -0.1498 0.1328 0.0781 0.066 Uiso 1 1 calc R U .
C11 C -0.1142(6) 0.1959(6) 0.03472(18) 0.0612(19) Uani 1 1 d . . .
H11 H -0.1754 0.1340 0.0251 0.073 Uiso 1 1 calc R U .
C12 C -0.0422(7) 0.2862(7) 0.0172(2) 0.075(2) Uani 1 1 d . . .
H12 H -0.0545 0.2873 -0.0043 0.089 Uiso 1 1 calc R U .
C13 C 0.0494(5) 0.3768(6) 0.0313(2) 0.0599(19) Uani 1 1 d . . .
H13 H 0.0992 0.4398 0.0194 0.072 Uiso 1 1 calc R U .
C14 C 0.0663(6) 0.3734(6) 0.06272(19) 0.0561(17) Uani 1 1 d . . .
H14 H 0.1290 0.4338 0.0723 0.067 Uiso 1 1 calc R U .
N1 N 0.0000 0.0000 0.26353(18) 0.0380(19) Uani 1 3 d S T P
N2 N 0.0386(3) 0.1866(4) 0.22666(13) 0.0404(11) Uani 1 1 d . U .
N3 N 0.0233(4) 0.2547(4) 0.17747(12) 0.0401(11) Uani 1 1 d . . .
H3A H 0.0696 0.3139 0.1668 0.048 Uiso 1 1 calc R U .
N4 N -0.0403(4) 0.1875(4) 0.12919(14) 0.0482(14) Uani 1 1 d . . .
H4A H -0.0783 0.1280 0.1176 0.058 Uiso 1 1 calc R U .
O1 O 0.0804(4) 0.3734(4) 0.12745(12) 0.0720(15) Uani 1 1 d . . .
O2 O 0.2370(5) 0.6669(5) 0.02275(16) 0.0850(18) Uani 1 1 d . . .
O3 O 0.3333 0.6667 0.0663(3) 0.118(4) Uani 1 3 d S T P
O4 O 0.0000 0.0000 0.0454(3) 0.126(5) Uani 1 3 d S T P
O5 O -0.1029(4) -0.0154(4) 0.09211(15) 0.0765(17) Uani 1 1 d . . .
O6 O 0.3333 0.6667 0.1667 0.102(11) Uani 0.5 6 d S T P
S1 S -0.13369(11) 0.04177(12) 0.17356(4) 0.0417(5) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.03322(8) 0.0525(8) Uani 1 3 d S T P
Cl2 Cl 0.0000 0.0000 0.08153(11) 0.0767(11) Uani 1 3 d S T P
Cd1 Cd 0.0000 0.0000 0.20809(2) 0.0340(4) Uani 1 3 d S T P
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'
Cl Cl 0.1484 0.1585 '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 C1 C2 114.7(5) . .
N2 C2 C3 119.7(6) . .
N2 C2 C1 116.4(6) . .
C3 C2 C1 123.4(7) . .
C4 C3 C2 120.4(7) . .
C3 C4 C5 120.4(6) . .
C6 C5 C4 118.3(6) . .
N2 C6 C5 121.7(6) . .
N2 C6 N3 117.4(5) . .
C5 C6 N3 120.7(5) . .
N3 C7 N4 114.7(6) . .
N3 C7 S1 127.2(6) . .
N4 C7 S1 118.1(4) . .
O1 C8 N4 121.2(7) . .
O1 C8 C9 121.1(6) . .
N4 C8 C9 117.7(5) . .
C14 C9 C10 119.8(7) . .
C14 C9 C8 118.4(6) . .
C10 C9 C8 121.8(6) . .
C11 C10 C9 120.1(6) . .
C10 C11 C12 120.4(7) . .
C11 C12 C13 119.9(8) . .
C14 C13 C12 119.3(7) . .
C9 C14 C13 120.6(7) . .
C1 N1 C1 110.4(4) 3 .
C1 N1 C1 110.4(4) 3 2
C1 N1 C1 110.4(4) . 2
C1 N1 Cd1 108.5(4) 3 .
C1 N1 Cd1 108.5(4) . .
C1 N1 Cd1 108.5(4) 2 .
C6 N2 C2 119.5(5) . .
C6 N2 Cd1 128.1(4) . .
C2 N2 Cd1 112.1(4) . .
C7 N3 C6 129.6(6) . .
C8 N4 C7 129.0(6) . .
C7 S1 Cd1 100.7(2) . .
O2 Cl1 O2 110.2(3) . 2_665
O2 Cl1 O2 110.2(3) . 3_565
O2 Cl1 O2 110.2(3) 2_665 3_565
O2 Cl1 O3 108.7(3) . .
O2 Cl1 O3 108.7(3) 2_665 .
O2 Cl1 O3 108.7(3) 3_565 .
O5 Cl2 O5 110.0(3) 3 2
O5 Cl2 O5 110.0(3) 3 .
O5 Cl2 O5 110.0(3) 2 .
O5 Cl2 O4 108.9(3) 3 .
O5 Cl2 O4 108.9(3) 2 .
O5 Cl2 O4 108.9(3) . .
N1 Cd1 N2 71.26(13) . 2
N1 Cd1 N2 71.26(13) . 3
N2 Cd1 N2 110.19(13) 2 3
N1 Cd1 N2 71.26(13) . .
N2 Cd1 N2 110.19(13) 2 .
N2 Cd1 N2 110.19(13) 3 .
N1 Cd1 S1 124.13(4) . .
N2 Cd1 S1 79.08(11) 2 .
N2 Cd1 S1 164.52(14) 3 .
N2 Cd1 S1 76.50(12) . .
N1 Cd1 S1 124.13(4) . 2
N2 Cd1 S1 76.50(12) 2 2
N2 Cd1 S1 79.08(11) 3 2
N2 Cd1 S1 164.52(14) . 2
S1 Cd1 S1 91.59(5) . 2
N1 Cd1 S1 124.13(4) . 3
N2 Cd1 S1 164.52(14) 2 3
N2 Cd1 S1 76.50(12) 3 3
N2 Cd1 S1 79.08(11) . 3
S1 Cd1 S1 91.59(5) . 3
S1 Cd1 S1 91.59(5) 2 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.447(6) .
C1 C2 1.490(8) .
C2 N2 1.386(9) .
C2 C3 1.388(9) .
C3 C4 1.359(9) .
C4 C5 1.393(10) .
C5 C6 1.388(8) .
C6 N2 1.353(7) .
C6 N3 1.433(8) .
C7 N3 1.312(7) .
C7 N4 1.393(9) .
C7 S1 1.651(7) .
C8 O1 1.257(7) .
C8 N4 1.347(8) .
C8 C9 1.483(10) .
C9 C14 1.375(9) .
C9 C10 1.393(9) .
C10 C11 1.374(10) .
C11 C12 1.374(10) .
C12 C13 1.404(10) .
C13 C14 1.383(10) .
N1 C1 1.447(6) 3
N1 C1 1.447(6) 2
N1 Cd1 2.398(8) .
N2 Cd1 2.500(5) .
O2 Cl1 1.413(5) .
O3 Cl1 1.433(13) .
O4 Cl2 1.564(15) .
O5 Cl2 1.411(5) .
S1 Cd1 2.6617(16) .
Cl1 O2 1.413(5) 2_665
Cl1 O2 1.413(6) 3_565
Cl2 O5 1.411(5) 3
Cl2 O5 1.411(5) 2
Cd1 N2 2.500(5) 2
Cd1 N2 2.500(5) 3
Cd1 S1 2.6617(16) 2
Cd1 S1 2.6617(16) 3
