#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:55:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180363 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/32/7203207.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_7203207
loop_
_publ_author_name
'Gale, Philip A.'
'Light, Mark E.'
'Quesada, Roberto'
_publ_section_title
;
 Tetrakis(thiourea)platinum(ii) oxocarbodianions salts as molecular
 building blocks for the synthesis of hydrogen bonded networks in the
 solid state
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              178
_journal_paper_doi               10.1039/b516238f
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C16 H40 N8 O8 Pt S8'
_chemical_formula_weight         924.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3461(14)
_cell_length_b                   10.1444(6)
_cell_length_c                   11.1430(11)
_cell_measurement_reflns_used    2395
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1847.7(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17029
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.295
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Slab
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.598
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.458(19)
_refine_ls_extinction_coef       0.0032(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0538
_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)+(0.0813P)²+9.8254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                3509
_reflns_number_total             4206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516238f.txt
_cod_data_source_block           2005sot0432
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21212
_cod_database_code               7203207
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.5000 0.0000 1.06114(4) 0.03540(18) Uani 1 2 d S . .
S1 S 0.39909(15) 0.0092(7) 0.9149(2) 0.0502(8) Uani 1 1 d . . .
S2 S 0.39918(14) 0.0107(7) 1.2071(2) 0.0502(8) Uani 1 1 d . . .
N2 N 0.4559(6) 0.2533(9) 0.8799(7) 0.044(2) Uani 1 1 d U . .
H2A H 0.4577 0.3289 0.8413 0.053 Uiso 1 1 calc R . .
H2B H 0.4858 0.2416 0.9448 0.053 Uiso 1 1 calc R . .
N1 N 0.3630(6) 0.1750(11) 0.7425(8) 0.052(2) Uani 1 1 d U . .
H1A H 0.3650 0.2507 0.7042 0.063 Uiso 1 1 calc R . .
H1B H 0.3312 0.1113 0.7161 0.063 Uiso 1 1 calc R . .
N3 N 0.4605(6) 0.2504(10) 1.2495(8) 0.052(2) Uani 1 1 d U . .
H3A H 0.4605 0.3267 1.2869 0.063 Uiso 1 1 calc R . .
H3B H 0.4936 0.2372 1.1884 0.063 Uiso 1 1 calc R . .
C1 C 0.4080(6) 0.1568(11) 0.8404(8) 0.042(2) Uani 1 1 d U . .
C2 C 0.4119(6) 0.1576(10) 1.2843(10) 0.044(2) Uani 1 1 d U . .
O1 O 0.5000 0.5000 0.3603(7) 0.066(3) Uani 1 2 d SU . .
O3 O 0.5000 0.5000 0.7700(7) 0.066(3) Uani 1 2 d SU . .
C5 C 0.5000 0.5000 0.6577(12) 0.062(4) Uani 1 2 d SU . .
O2 O 0.3882(6) 0.3632(9) 0.5644(8) 0.065(2) Uani 1 1 d U . .
N4 N 0.3609(7) 0.1756(9) 1.3775(10) 0.061(3) Uani 1 1 d U . .
H4A H 0.3602 0.2515 1.4157 0.073 Uiso 1 1 calc R . .
H4B H 0.3281 0.1115 1.4002 0.073 Uiso 1 1 calc R . .
C4 C 0.4502(10) 0.4390(11) 0.5625(11) 0.064(3) Uani 1 1 d U . .
C3 C 0.5000 0.5000 0.4727(10) 0.051(3) Uani 1 2 d SU . .
S3 S 0.3346(2) 0.6637(4) 0.0607(4) 0.0769(10) Uani 1 1 d D . .
O4 O 0.4221(5) 0.7069(9) 0.0616(8) 0.074(3) Uani 1 1 d DU . .
C6 C 0.3145(9) 0.6274(19) -0.0865(13) 0.099(5) Uani 1 1 d DU . .
H6A H 0.3189 0.7078 -0.1349 0.149 Uiso 1 1 calc R . .
H6B H 0.2590 0.5916 -0.0934 0.149 Uiso 1 1 calc R . .
H6C H 0.3540 0.5620 -0.1154 0.149 Uiso 1 1 calc R . .
C7 C 0.3375(7) 0.5027(14) 0.1159(14) 0.087(4) Uani 1 1 d DU . .
H7A H 0.3795 0.4524 0.0729 0.131 Uiso 1 1 calc R . .
H7B H 0.2841 0.4608 0.1042 0.131 Uiso 1 1 calc R . .
H7C H 0.3507 0.5044 0.2017 0.131 Uiso 1 1 calc R . .
S4 S 0.1695(5) 0.3444(6) 0.4130(6) 0.151(3) Uani 1 1 d D . .
O5 O 0.1913(6) 0.4867(10) 0.4321(9) 0.105(4) Uani 1 1 d DU . .
C8 C 0.0660(11) 0.346(2) 0.397(2) 0.164(10) Uani 1 1 d DU . .
H8A H 0.0418 0.4018 0.4594 0.246 Uiso 1 1 calc R . .
H8B H 0.0449 0.2557 0.4054 0.246 Uiso 1 1 calc R . .
H8C H 0.0517 0.3802 0.3179 0.246 Uiso 1 1 calc R . .
C9 C 0.1743(9) 0.2646(14) 0.5517(12) 0.082(4) Uani 1 1 d DU . .
H9A H 0.2190 0.3021 0.5994 0.122 Uiso 1 1 calc R . .
H9B H 0.1842 0.1704 0.5391 0.122 Uiso 1 1 calc R . .
H9C H 0.1225 0.2767 0.5944 0.122 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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'
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
_geom_angle_publ_flag
S2 Pt1 S2 90.90(13) 2_655 . ?
S2 Pt1 S1 89.15(9) 2_655 2_655 ?
S2 Pt1 S1 179.6(3) . 2_655 ?
S2 Pt1 S1 179.6(3) 2_655 . ?
S2 Pt1 S1 89.15(9) . . ?
S1 Pt1 S1 90.80(13) 2_655 . ?
C1 S1 Pt1 108.3(4) . . ?
C2 S2 Pt1 107.6(4) . . ?
N1 C1 N2 119.7(10) . . ?
N1 C1 S1 118.1(9) . . ?
N2 C1 S1 122.2(8) . . ?
N3 C2 N4 121.0(10) . . ?
N3 C2 S2 123.5(8) . . ?
N4 C2 S2 115.2(9) . . ?
O3 C5 C4 136.0(7) . 2_665 ?
O3 C5 C4 136.0(7) . . ?
C4 C5 C4 87.9(15) 2_665 . ?
O2 C4 C3 136.5(11) . . ?
O2 C4 C5 133.0(12) . . ?
C3 C4 C5 90.5(11) . . ?
O1 C3 C4 134.4(7) . 2_665 ?
O1 C3 C4 134.4(7) . . ?
C4 C3 C4 91.2(13) 2_665 . ?
O4 S3 C6 104.7(6) . . ?
O4 S3 C7 104.2(6) . . ?
C6 S3 C7 98.1(8) . . ?
O5 S4 C8 104.1(9) . . ?
O5 S4 C9 108.1(7) . . ?
C8 S4 C9 98.0(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 S2 2.318(2) 2_655 ?
Pt1 S2 2.318(2) . ?
Pt1 S1 2.320(2) 2_655 ?
Pt1 S1 2.320(2) . ?
S1 C1 1.718(13) . ?
S2 C2 1.734(12) . ?
N2 C1 1.329(14) . ?
N1 C1 1.329(13) . ?
N3 C2 1.291(15) . ?
C2 N4 1.345(14) . ?
O1 C3 1.252(15) . ?
O3 C5 1.252(15) . ?
C5 C4 1.472(16) 2_665 ?
C5 C4 1.472(16) . ?
O2 C4 1.273(17) . ?
C4 C3 1.431(18) . ?
C3 C4 1.431(18) 2_665 ?
S3 O4 1.496(8) . ?
S3 C6 1.712(14) . ?
S3 C7 1.747(12) . ?
S4 O5 1.502(10) . ?
S4 C8 1.701(15) . ?
S4 C9 1.746(12) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O3 0.88 2.03 2.878(9) 161.4 .
N1 H1A O2 0.88 1.97 2.785(13) 153.9 .
N2 H2B O4 0.88 2.06 2.870(12) 153.0 2_666
N3 H3B O4 0.88 2.05 2.873(13) 154.6 2_666
N3 H3A O1 0.88 2.04 2.891(10) 161.3 1_556
N4 H4A O2 0.88 2.06 2.857(13) 150.3 1_556
N1 H1B O5 0.88 2.11 2.867(13) 143.5 3_546
N4 H4B O5 0.88 2.28 2.984(16) 137.0 3_547
