#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/88/2018800.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018800
loop_
_publ_author_name
'Ozawa, Yoshiki'
'Kim, Misa'
'Toriumi, Koshiro'
_publ_section_title
;
 A one-dimensional platinum mixed-valence complex with bridging
 thiocyanate S atoms:
 [[PtII(en)₂](μ-SCN)[PtIV(en)₂](μ-SCN)](ClO₄)₄ (en is
 ethane-1,2-diamine)
;
_journal_coeditor_code           WQ3023
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              146
_journal_page_last               149
_journal_paper_doi               10.1107/S0108270113000541
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pt2 (N C S)2 (C2 H8 N2)4] (Cl O4)4'
_chemical_formula_moiety         'C10 H32 N10 Pt2 S2 4+, 4(Cl O4 -)'
_chemical_formula_sum            'C10 H32 Cl4 N10 O16 Pt2 S2'
_chemical_formula_weight         1144.56
_chemical_name_systematic
;
catena-Poly[[[bis(ethane-1,2-diamine-
κ²N,N')platinum(II)]-μ-thiocyanato-κ²S:S-
[bis(ethane-1,2-diamine-κ²N,N')platinum(IV)]-μ-
thiocyanato-κ²S:S] tetrakis(perchlorate)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.944(4)
_cell_angle_beta                 91.574(4)
_cell_angle_gamma                113.765(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0535(13)
_cell_length_b                   9.6033(14)
_cell_length_c                   9.6034(14)
_cell_measurement_reflns_used    7324
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.725
_cell_measurement_theta_min      3.08
_cell_volume                     730.11(19)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction
;
CrystalClear (Rigaku, 2008) and SORTAV (Blessing, 1995)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae et al., 2008)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'fixed Χ-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku SCX-MINI'
_diffrn_measurement_method       'ω oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7690
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    10.167
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.202
_refine_diff_density_min         -2.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0232P)²+0.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                3014
_reflns_number_total             3333
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wq3023.cif
_cod_data_source_block           I
_cod_original_cell_volume        730.11(18)
_cod_database_code               2018800
_cod_database_fobs_code          2018800
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pt Pt1 0.5 0.5 0.5 0.01129(8) Uani d S 1 2
S S1 0.50034(12) 0.28326(12) 0.30922(11) 0.0220(2) Uani d . 1 1
C C1 0.6993(5) 0.3479(5) 0.2941(4) 0.0211(8) Uani d . 1 1
N N1 0.8344(5) 0.3900(5) 0.2865(4) 0.0319(9) Uani d . 1 1
N N2 0.2579(4) 0.3527(4) 0.4900(4) 0.0163(7) Uani d . 1 1
H H2A 0.2462 0.2533 0.4826 0.024 Uiso calc R 1 1
H H2B 0.2208 0.3877 0.5716 0.024 Uiso calc R 1 1
N N3 0.4087(5) 0.5759(5) 0.3502(4) 0.0177(8) Uani d . 1 1
H H3A 0.4566 0.6829 0.3747 0.027 Uiso calc R 1 1
H H3B 0.4307 0.5376 0.2614 0.027 Uiso calc R 1 1
C C2 0.1634(5) 0.3522(5) 0.3603(4) 0.0216(8) Uani d . 1 1
H H2C 0.0489 0.3161 0.3713 0.032 Uiso calc R 1 1
H H2D 0.173 0.2802 0.2732 0.032 Uiso calc R 1 1
C C3 0.2297(5) 0.5193(6) 0.3466(5) 0.0202(9) Uani d . 1 1
H H3C 0.1802 0.5192 0.2557 0.03 Uiso calc R 1 1
H H3D 0.2058 0.5887 0.4265 0.03 Uiso calc R 1 1
Pt Pt2 0.5 0 0 0.01364(8) Uani d S 1 2
N N4 0.2652(5) -0.1248(4) 0.0261(4) 0.0175(7) Uani d . 1 1
H H4A 0.2286 -0.2271 -0.028 0.026 Uiso calc R 1 1
H H4B 0.2601 -0.1221 0.1201 0.026 Uiso calc R 1 1
N N5 0.3959(5) 0.0902(5) -0.1229(4) 0.0196(8) Uani d . 1 1
H H5A 0.419 0.1921 -0.0748 0.029 Uiso calc R 1 1
H H5B 0.437 0.0883 -0.2072 0.029 Uiso calc R 1 1
C C4 0.1620(5) -0.0524(5) -0.0204(5) 0.0245(9) Uani d . 1 1
H H4C 0.173 0.0405 0.057 0.037 Uiso calc R 1 1
H H4D 0.0482 -0.1284 -0.0413 0.037 Uiso calc R 1 1
C C5 0.2157(6) -0.0057(6) -0.1536(6) 0.0242(10) Uani d . 1 1
H H5C 0.1876 -0.0998 -0.2359 0.036 Uiso calc R 1 1
H H5D 0.1621 0.0566 -0.177 0.036 Uiso calc R 1 1
Cl Cl1 0.22426(15) -0.05757(13) 0.42496(13) 0.0256(2) Uani d . 1 1
O O1 0.3261(6) -0.1202(5) 0.3461(5) 0.0440(11) Uani d . 1 1
O O2 0.3205(6) 0.0737(5) 0.5516(4) 0.0426(10) Uani d . 1 1
O O3 0.1549(4) 0.0025(4) 0.3318(4) 0.0424(9) Uani d . 1 1
O O4 0.1009(5) -0.1785(4) 0.4701(4) 0.0470(10) Uani d . 1 1
Cl Cl2 0.24808(14) 0.41662(12) 0.94696(12) 0.0206(2) Uani d . 1 1
O O5 0.3090(5) 0.3777(5) 0.8119(4) 0.0353(9) Uani d . 1 1
O O6 0.3237(5) 0.5855(4) 1.0133(4) 0.0364(9) Uani d . 1 1
O O7 0.2902(4) 0.3417(4) 1.0441(3) 0.0377(8) Uani d . 1 1
O O8 0.0767(4) 0.3621(5) 0.9211(5) 0.0471(10) Uani d . 1 1
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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Pt1 N2 . 2_666 180
N2 Pt1 N3 . . 83.28(15)
N2 Pt1 N3 2_666 . 96.72(15)
N2 Pt1 N3 . 2_666 96.72(15)
N2 Pt1 N3 2_666 2_666 83.28(15)
N3 Pt1 N3 . 2_666 179.999(2)
N2 Pt1 S1 . 2_666 95.20(10)
N2 Pt1 S1 2_666 2_666 84.80(10)
N3 Pt1 S1 . 2_666 89.45(11)
N3 Pt1 S1 2_666 2_666 90.56(11)
N2 Pt1 S1 . . 84.80(10)
N2 Pt1 S1 2_666 . 95.20(10)
N3 Pt1 S1 . . 90.55(11)
N3 Pt1 S1 2_666 . 89.44(11)
S1 Pt1 S1 2_666 . 180
N2 Pt1 C2 . . 29.13(13)
N2 Pt1 C2 2_666 . 150.87(13)
N3 Pt1 C2 . . 55.17(13)
N3 Pt1 C2 2_666 . 124.83(13)
S1 Pt1 C2 2_666 . 100.82(9)
S1 Pt1 C2 . . 79.18(9)
N2 Pt1 C2 . 2_666 150.87(13)
N2 Pt1 C2 2_666 2_666 29.13(13)
N3 Pt1 C2 . 2_666 124.83(13)
N3 Pt1 C2 2_666 2_666 55.17(13)
S1 Pt1 C2 2_666 2_666 79.18(9)
S1 Pt1 C2 . 2_666 100.82(9)
C2 Pt1 C2 . 2_666 180.00(18)
N2 Pt1 C3 . 2_666 124.33(14)
N2 Pt1 C3 2_666 2_666 55.67(14)
N3 Pt1 C3 . 2_666 151.39(14)
N3 Pt1 C3 2_666 2_666 28.61(14)
S1 Pt1 C3 2_666 2_666 94.72(10)
S1 Pt1 C3 . 2_666 85.28(10)
C2 Pt1 C3 . 2_666 149.84(12)
C2 Pt1 C3 2_666 2_666 30.16(12)
N2 Pt1 C3 . . 55.67(14)
N2 Pt1 C3 2_666 . 124.33(14)
N3 Pt1 C3 . . 28.61(14)
N3 Pt1 C3 2_666 . 151.39(14)
S1 Pt1 C3 2_666 . 85.28(10)
S1 Pt1 C3 . . 94.72(10)
C2 Pt1 C3 . . 30.16(12)
C2 Pt1 C3 2_666 . 149.84(12)
C3 Pt1 C3 2_666 . 180
C1 S1 Pt1 . . 101.44(14)
C1 S1 Pt2 . . 77.77(13)
Pt1 S1 Pt2 . . 171.97(4)
N1 C1 S1 . . 178.3(4)
C2 N2 Pt1 . . 108.6(3)
C2 N2 H2A . . 110
Pt1 N2 H2A . . 110
C2 N2 H2B . . 110
Pt1 N2 H2B . . 110
H2A N2 H2B . . 108.3
C3 N3 Pt1 . . 109.7(3)
C3 N3 H3A . . 109.7
Pt1 N3 H3A . . 109.7
C3 N3 H3B . . 109.7
Pt1 N3 H3B . . 109.7
H3A N3 H3B . . 108.2
N2 C2 C3 . . 108.9(3)
N2 C2 Pt1 . . 42.25(18)
C3 C2 Pt1 . . 75.5(2)
N2 C2 H2C . . 109.9
C3 C2 H2C . . 109.9
Pt1 C2 H2C . . 147.8
N2 C2 H2D . . 109.9
C3 C2 H2D . . 109.9
Pt1 C2 H2D . . 98.7
H2C C2 H2D . . 108.3
N3 C3 C2 . . 107.4(4)
N3 C3 Pt1 . . 41.70(19)
C2 C3 Pt1 . . 74.3(2)
N3 C3 H3C . . 110.2
C2 C3 H3C . . 110.2
Pt1 C3 H3C . . 147.3
N3 C3 H3D . . 110.2
C2 C3 H3D . . 110.2
Pt1 C3 H3D . . 99.3
H3C C3 H3D . . 108.5
N4 Pt2 N4 . 2_655 180
N4 Pt2 N5 . 2_655 96.56(15)
N4 Pt2 N5 2_655 2_655 83.44(15)
N4 Pt2 N5 . . 83.44(15)
N4 Pt2 N5 2_655 . 96.56(15)
N5 Pt2 N5 2_655 . 180
N4 Pt2 C4 . 2_655 150.80(13)
N4 Pt2 C4 2_655 2_655 29.20(13)
N5 Pt2 C4 2_655 2_655 55.37(14)
N5 Pt2 C4 . 2_655 124.63(14)
N4 Pt2 C4 . . 29.20(13)
N4 Pt2 C4 2_655 . 150.80(13)
N5 Pt2 C4 2_655 . 124.63(14)
N5 Pt2 C4 . . 55.37(14)
C4 Pt2 C4 2_655 . 180
N4 Pt2 C5 . 2_655 124.56(14)
N4 Pt2 C5 2_655 2_655 55.44(14)
N5 Pt2 C5 2_655 2_655 28.82(14)
N5 Pt2 C5 . 2_655 151.18(14)
C4 Pt2 C5 2_655 2_655 29.88(13)
C4 Pt2 C5 . 2_655 150.12(13)
N4 Pt2 C5 . . 55.44(14)
N4 Pt2 C5 2_655 . 124.56(14)
N5 Pt2 C5 2_655 . 151.18(14)
N5 Pt2 C5 . . 28.82(14)
C4 Pt2 C5 2_655 . 150.12(13)
C4 Pt2 C5 . . 29.88(13)
C5 Pt2 C5 2_655 . 180
N4 Pt2 S1 . . 84.11(10)
N4 Pt2 S1 2_655 . 95.89(10)
N5 Pt2 S1 2_655 . 91.01(11)
N5 Pt2 S1 . . 88.99(11)
C4 Pt2 S1 2_655 . 102.49(9)
C4 Pt2 S1 . . 77.51(9)
C5 Pt2 S1 2_655 . 87.56(11)
C5 Pt2 S1 . . 92.44(11)
N4 Pt2 S1 . 2_655 95.89(10)
N4 Pt2 S1 2_655 2_655 84.11(10)
N5 Pt2 S1 2_655 2_655 88.99(11)
N5 Pt2 S1 . 2_655 91.01(11)
C4 Pt2 S1 2_655 2_655 77.51(9)
C4 Pt2 S1 . 2_655 102.49(9)
C5 Pt2 S1 2_655 2_655 92.44(11)
C5 Pt2 S1 . 2_655 87.56(11)
S1 Pt2 S1 . 2_655 180
C4 N4 Pt2 . . 108.9(3)
C4 N4 H4A . . 109.9
Pt2 N4 H4A . . 109.9
C4 N4 H4B . . 109.9
Pt2 N4 H4B . . 109.9
H4A N4 H4B . . 108.3
C5 N5 Pt2 . . 109.9(3)
C5 N5 H5A . . 109.7
Pt2 N5 H5A . . 109.7
C5 N5 H5B . . 109.7
Pt2 N5 H5B . . 109.7
H5A N5 H5B . . 108.2
N4 C4 C5 . . 108.8(3)
N4 C4 Pt2 . . 41.87(18)
C5 C4 Pt2 . . 75.8(2)
N4 C4 H4C . . 109.9
C5 C4 H4C . . 109.9
Pt2 C4 H4C . . 98.7
N4 C4 H4D . . 109.9
C5 C4 H4D . . 109.9
Pt2 C4 H4D . . 147.6
H4C C4 H4D . . 108.3
N5 C5 C4 . . 107.7(4)
N5 C5 Pt2 . . 41.3(2)
C4 C5 Pt2 . . 74.4(2)
N5 C5 H5C . . 110.2
C4 C5 H5C . . 110.2
Pt2 C5 H5C . . 100.3
N5 C5 H5D . . 110.2
C4 C5 H5D . . 110.2
Pt2 C5 H5D . . 146.4
H5C C5 H5D . . 108.5
O4 Cl1 O1 . . 109.9(3)
O4 Cl1 O3 . . 111.4(2)
O1 Cl1 O3 . . 108.0(2)
O4 Cl1 O2 . . 109.4(2)
O1 Cl1 O2 . . 110.2(3)
O3 Cl1 O2 . . 108.0(2)
O8 Cl2 O6 . . 109.9(3)
O8 Cl2 O5 . . 110.2(3)
O6 Cl2 O5 . . 109.6(2)
O8 Cl2 O7 . . 109.9(2)
O6 Cl2 O7 . . 108.6(2)
O5 Cl2 O7 . . 108.7(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pt1 N2 . 2.057(4)
Pt1 N2 2_666 2.057(4)
Pt1 N3 . 2.060(4)
Pt1 N3 2_666 2.060(4)
Pt1 S1 2_666 2.3933(10)
Pt1 S1 . 2.3933(10)
Pt1 C2 . 2.900(4)
Pt1 C2 2_666 2.900(4)
Pt1 C3 2_666 2.916(5)
Pt1 C3 . 2.916(5)
S1 C1 . 1.676(4)
S1 Pt2 . 3.4705(11)
C1 N1 . 1.135(5)
N2 C2 . 1.490(5)
N2 H2A . 0.9
N2 H2B . 0.9
N3 C3 . 1.483(6)
N3 H3A . 0.9
N3 H3B . 0.9
C2 C3 . 1.513(6)
C2 H2C . 0.97
C2 H2D . 0.97
C3 H3C . 0.97
C3 H3D . 0.97
Pt2 N4 . 2.037(4)
Pt2 N4 2_655 2.037(4)
Pt2 N5 2_655 2.039(4)
Pt2 N5 . 2.039(4)
Pt2 C4 2_655 2.886(4)
Pt2 C4 . 2.886(4)
Pt2 C5 2_655 2.905(5)
Pt2 C5 . 2.905(5)
Pt2 S1 2_655 3.4705(11)
N4 C4 . 1.489(5)
N4 H4A . 0.9
N4 H4B . 0.9
N5 C5 . 1.489(6)
N5 H5A . 0.9
N5 H5B . 0.9
C4 C5 . 1.493(6)
C4 H4C . 0.97
C4 H4D . 0.97
C5 H5C . 0.97
C5 H5D . 0.97
Cl1 O4 . 1.423(4)
Cl1 O1 . 1.427(4)
Cl1 O3 . 1.434(3)
Cl1 O2 . 1.447(4)
Cl2 O8 . 1.414(4)
Cl2 O6 . 1.433(4)
Cl2 O5 . 1.443(4)
Cl2 O7 . 1.443(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2A O2 . 0.9 2.32 3.142(6) 152.4 ?
N2 H2A O3 . 0.9 2.26 3.041(5) 144.7 y
N2 H2B O5 . 0.9 2.46 3.045(5) 123.1 y
N2 H2B N1 2_666 0.9 2.46 3.231(5) 143.7 ?
N3 H3B O5 2_666 0.9 2.36 2.969(6) 125.3 y
N3 H3B O7 1_554 0.9 2.33 3.053(5) 137.8 y
N3 H3A O2 2_666 0.9 2.3 3.132(6) 153.1 ?
N4 H4A O6 1_544 0.9 2.39 3.008(5) 125.6 y
N4 H4A N1 2_655 0.9 2.48 3.220(5) 140.2 ?
N4 H4B O1 . 0.9 2.23 3.093(6) 161 ?
N4 H4B O3 . 0.9 2.5 3.225(5) 138.2 ?
N5 H5B O2 1_554 0.9 2.46 3.131(5) 131.1 ?
N5 H5B O1 2_655 0.9 2.51 3.324(6) 150.2 ?
N5 H5A O6 2_666 0.9 2.37 3.007(5) 128.1 y
N5 H5A O7 1_554 0.9 2.3 3.044(5) 139.5 y
