#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:06:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178835 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/89/4108962.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_4108962
loop_
_publ_author_name
'Hiroaki Iguchi'
'Shinya Takaishi'
'Takashi Kajiwara'
'Hitoshi Miyasaka'
'Masahiro Yamashita'
'Hiroyuki Matsuzaki'
'Hiroshi Okamoto'
_publ_section_title
;
 Mixed Charge-Ordering State of MMX-Type Quasi-One-Dimensional
 Iodide-Bridged Platinum Complexes with Binary Countercations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17668
_journal_page_last               17669
_journal_paper_doi               10.1021/ja807901p
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C4 H30 I K2 N2 O24 P8 Pt2'
_chemical_formula_weight         1333.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           104
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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            4
_cell_length_a                   13.4130(16)
_cell_length_b                   13.4130(16)
_cell_length_c                   17.257(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3104.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29282
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    10.770
_exptl_absorpt_correction_T_max  0.430546
_exptl_absorpt_correction_T_min  0.343422
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.393(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0233
_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)+(0.0249P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                2947
_reflns_number_total             3584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807901p_si_001.cif
_cod_data_source_block           2_menc3
_cod_database_code               4108962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, 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
Pt1 Pt 1.0000 1.0000 0.824155(12) 0.00683(7) Uani 1 4 d S
Pt2 Pt 1.0000 1.0000 0.658030(17) 0.00655(6) Uani 1 4 d S
Pt3 Pt 1.0000 1.0000 0.314670(13) 0.00676(7) Uani 1 4 d S
Pt4 Pt 1.0000 1.0000 0.155492(18) 0.00658(6) Uani 1 4 d S
I1 I 1.0000 1.0000 0.99616(3) 0.01308(11) Uani 1 4 d S
I2 I 1.0000 1.0000 0.47688(3) 0.01284(12) Uani 1 4 d S
P1 P 0.92741(7) 0.84189(7) 0.82719(5) 0.0089(2) Uani 1 1 d .
P2 P 0.89770(7) 0.86034(7) 0.65651(7) 0.0086(2) Uani 1 1 d .
P3 P 0.88114(8) 0.87222(8) 0.31801(5) 0.0095(2) Uani 1 1 d .
P4 P 0.91113(7) 0.84907(7) 0.15025(6) 0.0107(2) Uani 1 1 d .
O1 O 0.82593(18) 0.83711(18) 0.87370(15) 0.0146(7) Uani 1 1 d .
O2 O 0.99036(19) 0.75657(19) 0.85739(14) 0.0157(7) Uani 1 1 d .
O3 O 0.8951(2) 0.80716(18) 0.74090(16) 0.0194(7) Uani 1 1 d .
O4 O 0.79017(19) 0.87638(19) 0.63334(15) 0.0152(7) Uani 1 1 d .
O5 O 0.9375(2) 0.77227(19) 0.60335(15) 0.0164(7) Uani 1 1 d .
O6 O 0.77720(19) 0.90041(18) 0.34321(16) 0.0152(7) Uani 1 1 d .
O7 O 0.91376(18) 0.78089(19) 0.37034(15) 0.0128(7) Uani 1 1 d .
O8 O 0.8687(2) 0.8193(2) 0.23408(17) 0.0235(8) Uani 1 1 d .
O9 O 0.8123(2) 0.8573(2) 0.10102(17) 0.0216(8) Uani 1 1 d .
O10 O 0.9694(2) 0.7590(2) 0.12202(16) 0.0197(8) Uani 1 1 d .
N1 N 0.6436(3) 0.8828(3) 0.7403(3) 0.0627(13) Uani 1 1 d .
H2 H 0.6742 0.9179 0.7787 0.094 Uiso 1 1 calc R
H3 H 0.6897 0.8632 0.7048 0.094 Uiso 1 1 calc R
H4 H 0.6134 0.8281 0.7610 0.094 Uiso 1 1 calc R
C1 C 0.5704(3) 0.9444(4) 0.7035(3) 0.0409(15) Uani 1 1 d .
C2 C 0.4828(6) 0.9886(9) 0.7505(5) 0.021(3) Uani 0.50 1 d P
C3 C 0.5162(7) 1.0201(10) 0.8319(4) 0.034(4) Uani 0.50 1 d P
K1 K 0.71610(5) 0.73177(5) 0.98946(6) 0.01396(17) Uani 1 1 d .
O11 O 0.56645(19) 0.87592(17) 1.00386(16) 0.0226(8) Uani 1 1 d .
O12 O 0.92247(16) 0.64977(15) 0.99074(19) 0.0156(6) 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
P1 Pt1 P1 89.971(1) . 4_575
P1 Pt1 P1 177.43(5) . 2_775
P1 Pt1 P1 89.971(1) 4_575 2_775
P1 Pt1 P1 89.971(1) . 3_755
P1 Pt1 P1 177.43(5) 4_575 3_755
P1 Pt1 P1 89.971(1) 2_775 3_755
P1 Pt1 Pt2 91.29(2) . .
P1 Pt1 Pt2 91.29(2) 4_575 .
P1 Pt1 Pt2 91.29(2) 2_775 .
P1 Pt1 Pt2 91.29(2) 3_755 .
P1 Pt1 I1 88.71(2) . .
P1 Pt1 I1 88.71(2) 4_575 .
P1 Pt1 I1 88.71(2) 2_775 .
P1 Pt1 I1 88.71(2) 3_755 .
Pt2 Pt1 I1 180.0 . .
P2 Pt2 P2 178.70(6) . 2_775
P2 Pt2 P2 89.993(1) . 3_755
P2 Pt2 P2 89.993(1) 2_775 3_755
P2 Pt2 P2 89.993(1) . 4_575
P2 Pt2 P2 89.993(1) 2_775 4_575
P2 Pt2 P2 178.70(6) 3_755 4_575
P2 Pt2 Pt1 90.65(3) . .
P2 Pt2 Pt1 90.65(3) 2_775 .
P2 Pt2 Pt1 90.65(3) 3_755 .
P2 Pt2 Pt1 90.65(3) 4_575 .
P2 Pt2 I2 89.35(3) . .
P2 Pt2 I2 89.35(3) 2_775 .
P2 Pt2 I2 89.35(3) 3_755 .
P2 Pt2 I2 89.35(3) 4_575 .
Pt1 Pt2 I2 180.0 . .
P3 Pt3 P3 177.18(5) . 2_775
P3 Pt3 P3 89.965(1) . 4_575
P3 Pt3 P3 89.965(1) 2_775 4_575
P3 Pt3 P3 89.965(1) . 3_755
P3 Pt3 P3 89.965(1) 2_775 3_755
P3 Pt3 P3 177.18(5) 4_575 3_755
P3 Pt3 Pt4 91.41(2) . .
P3 Pt3 Pt4 91.41(2) 2_775 .
P3 Pt3 Pt4 91.41(2) 4_575 .
P3 Pt3 Pt4 91.41(2) 3_755 .
P3 Pt3 I2 88.59(2) . .
P3 Pt3 I2 88.59(2) 2_775 .
P3 Pt3 I2 88.59(2) 4_575 .
P3 Pt3 I2 88.59(2) 3_755 .
Pt4 Pt3 I2 180.0 . .
P4 Pt4 P4 89.915(2) . 4_575
P4 Pt4 P4 175.59(6) . 2_775
P4 Pt4 P4 89.915(2) 4_575 2_775
P4 Pt4 P4 89.915(2) . 3_755
P4 Pt4 P4 175.59(6) 4_575 3_755
P4 Pt4 P4 89.915(2) 2_775 3_755
P4 Pt4 Pt3 92.20(3) . .
P4 Pt4 Pt3 92.20(3) 4_575 .
P4 Pt4 Pt3 92.20(3) 2_775 .
P4 Pt4 Pt3 92.20(3) 3_755 .
P4 Pt4 I1 87.80(3) . 1_554
P4 Pt4 I1 87.80(3) 4_575 1_554
P4 Pt4 I1 87.80(3) 2_775 1_554
P4 Pt4 I1 87.80(3) 3_755 1_554
Pt3 Pt4 I1 180.0 . 1_554
Pt4 I1 Pt1 180.0 1_556 .
Pt3 I2 Pt2 180.0 . .
O2 P1 O1 105.93(14) . .
O2 P1 O3 104.37(14) . .
O1 P1 O3 102.98(15) . .
O2 P1 Pt1 117.50(11) . .
O1 P1 Pt1 114.03(10) . .
O3 P1 Pt1 110.63(10) . .
O4 P2 O5 105.89(15) . .
O4 P2 O3 106.23(15) . .
O5 P2 O3 101.47(14) . .
O4 P2 Pt2 116.86(11) . .
O5 P2 Pt2 114.07(11) . .
O3 P2 Pt2 110.93(10) . .
O4 P2 K1 49.76(10) . 8_664
O5 P2 K1 58.39(10) . 8_664
O3 P2 K1 126.65(10) . 8_664
Pt2 P2 K1 122.41(4) . 8_664
O6 P3 O7 106.55(15) . .
O6 P3 O8 105.80(15) . .
O7 P3 O8 101.50(15) . .
O6 P3 Pt3 116.93(11) . .
O7 P3 Pt3 113.09(10) . .
O8 P3 Pt3 111.60(11) . .
O6 P3 K1 56.34(10) . 8_664
O7 P3 K1 51.73(10) . 8_664
O8 P3 K1 123.92(11) . 8_664
Pt3 P3 K1 123.96(4) . 8_664
O10 P4 O9 108.37(17) . .
O10 P4 O8 105.89(16) . .
O9 P4 O8 101.84(16) . .
O10 P4 Pt4 115.87(12) . .
O9 P4 Pt4 112.71(12) . .
O8 P4 Pt4 111.04(11) . .
P1 O1 K1 144.98(14) . .
P1 O3 P2 133.90(17) . .
P2 O4 K1 105.81(13) . 8_664
P2 O5 K1 94.88(12) . 8_664
P3 O6 K1 98.66(12) . 8_664
P3 O7 K1 102.26(12) . 8_664
P4 O8 P3 131.31(18) . .
P4 O9 K1 134.33(16) . 1_554
C2 C1 N1 117.4(5) 2_675 .
C2 C1 C2 20.9(7) 2_675 .
N1 C1 C2 120.6(5) . .
C2 C2 C1 94(2) 2_675 2_675
C2 C2 C3 92.2(5) 2_675 2_675
C1 C2 C3 129.3(9) 2_675 2_675
C2 C2 C3 66.7(5) 2_675 .
C1 C2 C3 120.0(9) 2_675 .
C3 C2 C3 26.8(9) 2_675 .
C2 C2 C1 65.2(17) 2_675 .
C1 C2 C1 109.1(6) 2_675 .
C3 C2 C1 119.0(8) 2_675 .
C3 C2 C1 111.4(6) . .
C3 C3 C2 86.6(7) 2_675 2_675
C3 C3 C2 66.5(5) 2_675 .
C2 C3 C2 21.1(7) 2_675 .
O4 K1 O11 71.04(8) 8_665 .
O4 K1 O7 125.37(8) 8_665 8_665
O11 K1 O7 123.39(8) . 8_665
O4 K1 O1 154.64(8) 8_665 .
O11 K1 O1 95.18(8) . .
O7 K1 O1 79.99(8) 8_665 .
O4 K1 O9 70.39(8) 8_665 1_556
O11 K1 O9 81.79(8) . 1_556
O7 K1 O9 152.32(8) 8_665 1_556
O1 K1 O9 86.95(8) . 1_556
O4 K1 O6 121.18(7) 8_665 8_665
O11 K1 O6 74.10(8) . 8_665
O7 K1 O6 50.48(7) 8_665 8_665
O1 K1 O6 72.37(8) . 8_665
O9 K1 O6 146.26(8) 1_556 8_665
O4 K1 O12 111.56(9) 8_665 .
O11 K1 O12 157.09(7) . .
O7 K1 O12 74.81(8) 8_665 .
O1 K1 O12 73.05(8) . .
O9 K1 O12 78.08(8) 1_556 .
O6 K1 O12 118.70(8) 8_665 .
O4 K1 O5 50.36(7) 8_665 8_665
O11 K1 O5 120.06(8) . 8_665
O7 K1 O5 87.32(7) 8_665 8_665
O1 K1 O5 143.51(7) . 8_665
O9 K1 O5 88.93(8) 1_556 8_665
O6 K1 O5 123.50(8) 8_665 8_665
O12 K1 O5 70.62(7) . 8_665
O4 K1 P2 24.43(6) 8_665 8_665
O11 K1 P2 93.40(6) . 8_665
O7 K1 P2 104.98(6) 8_665 8_665
O1 K1 P2 165.38(6) . 8_665
O9 K1 P2 82.58(7) 1_556 8_665
O6 K1 P2 121.52(6) 8_665 8_665
O12 K1 P2 94.73(6) . 8_665
O5 K1 P2 26.73(5) 8_665 8_665
O4 K1 P3 123.47(6) 8_665 8_665
O11 K1 P3 97.48(6) . 8_665
O7 K1 P3 26.01(5) 8_665 8_665
O1 K1 P3 78.40(6) . 8_665
O9 K1 P3 165.23(7) 1_556 8_665
O6 K1 P3 25.00(5) 8_665 8_665
O12 K1 P3 99.19(6) . 8_665
O5 K1 P3 103.97(6) 8_665 8_665
P2 K1 P3 112.17(3) 8_665 8_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.3341(10) .
Pt1 P1 2.3341(10) 4_575
Pt1 P1 2.3341(10) 2_775
Pt1 P1 2.3341(10) 3_755
Pt1 Pt2 2.8668(6) .
Pt1 I1 2.9683(8) .
Pt2 P2 2.3223(9) .
Pt2 P2 2.3223(9) 2_775
Pt2 P2 2.3223(9) 3_755
Pt2 P2 2.3223(9) 4_575
Pt2 I2 3.1261(8) .
Pt3 P3 2.3415(11) .
Pt3 P3 2.3415(11) 2_775
Pt3 P3 2.3415(11) 4_575
Pt3 P3 2.3415(11) 3_755
Pt3 Pt4 2.7469(6) .
Pt3 I2 2.7993(7) .
Pt4 P4 2.3510(10) .
Pt4 P4 2.3510(10) 4_575
Pt4 P4 2.3510(10) 2_775
Pt4 P4 2.3510(10) 3_755
Pt4 I1 2.7496(8) 1_554
I1 Pt4 2.7496(8) 1_556
P1 O2 1.515(3) .
P1 O1 1.582(3) .
P1 O3 1.619(3) .
P2 O4 1.512(3) .
P2 O5 1.588(3) .
P2 O3 1.622(3) .
P2 K1 3.5180(15) 8_664
P3 O6 1.508(3) .
P3 O7 1.584(3) .
P3 O8 1.621(3) .
P3 K1 3.5286(14) 8_664
P4 O10 1.518(3) .
P4 O9 1.578(3) .
P4 O8 1.605(3) .
O1 K1 2.856(3) .
O4 K1 2.791(3) 8_664
O5 K1 3.007(3) 8_664
O6 K1 2.971(3) 8_664
O7 K1 2.835(3) 8_664
O9 K1 2.865(3) 1_554
N1 C1 1.432(6) .
C1 C2 1.406(11) 2_675
C1 C2 1.546(10) .
C2 C2 0.553(17) 2_675
C2 C1 1.406(11) 2_675
C2 C3 1.408(11) 2_675
C2 C3 1.532(11) .
C3 C3 0.69(2) 2_675
C3 C2 1.408(11) 2_675
K1 O4 2.791(3) 8_665
K1 O11 2.798(3) .
K1 O7 2.835(3) 8_665
K1 O9 2.865(3) 1_556
K1 O6 2.971(3) 8_665
K1 O12 2.979(2) .
K1 O5 3.007(3) 8_665
K1 P2 3.5180(15) 8_665
K1 P3 3.5286(14) 8_665
