#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/66/4116602.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_4116602
loop_
_publ_author_name
'Tadashi Yamaguchi'
'Haruko Saito'
'Taro Maki'
'Tasuku Ito'
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
Tohoku University,Sendai  980-8578, JAPAN
;
_publ_contact_author_email       ' Ito@agnus.chem.tohoku.ac.jp '
_publ_contact_author_fax         ' +81 22 217 6548 '
_publ_contact_author_name        ' Tasuku ITO '
_publ_contact_author_phone       ' +81 22 217 6544 '
_publ_section_title
;
 Syntheses and Structures of Bridge and Chelate Isomers of
 Tetraplatinum(II) Cluster Complex with Diethyldithiophosphate Ion
 (Et2dtp) at In-Plane Sites, [Pt4(CH3COO)4(Et2dtp)4], and Their Mutual
 Isomerization via Cluster Core Rotation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10738
_journal_page_last               10742
_journal_paper_doi               10.1021/ja990596u
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C24 H52 O16 P4 Pt4 S8 '
_chemical_formula_sum            'C24 H52 O16 P4 Pt4 S8'
_chemical_formula_weight         1757.40
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             'Sun Dec 27 16:22:59 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.794(8)
_cell_length_b                   24.990(3)
_cell_length_c                   14.927(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.8
_cell_volume                     4772(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.00580
_diffrn_orient_matrix_UB_12      -0.03929
_diffrn_orient_matrix_UB_13      0.01166
_diffrn_orient_matrix_UB_21      -0.00284
_diffrn_orient_matrix_UB_22      -0.00708
_diffrn_orient_matrix_UB_23      -0.06589
_diffrn_orient_matrix_UB_31      0.07789
_diffrn_orient_matrix_UB_32      0.00267
_diffrn_orient_matrix_UB_33      -0.00327
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.352
_diffrn_reflns_av_sigmaI/netI    0.083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5508
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        -2.18
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.183
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3296.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       0.00018(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.477
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0192
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00006|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0374
_reflns_number_gt                4052
_reflns_number_total             5507
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja990596u_2.cif
_cod_data_source_block           '[Pt4(OAc)4(dtp)4]_fr.2'
_cod_original_cell_volume        4772(2)
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C24 H52 O16 P4 Pt4 S8 '
_cod_database_code               4116602
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,1/2+z
1/2+x,1/2-y,-z
-x,y,1/2-z
-x,-y,-z
1/2+x,1/2+y,1/2-z
1/2-x,1/2+y,z
x,-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_calc_flag
Pt(1) Pt -0.03265(3) 0.10178(1) 0.13555(2) 0.01563(8) Uani 1.00 d
Pt(2) Pt 0.13721(3) 0.12420(1) 0.22121(2) 0.01601(9) Uani 1.00 d
S(1) S 0.0539(2) 0.0865(1) -0.0094(2) 0.0261(7) Uani 1.00 d
S(2) S 0.2442(2) 0.1575(1) 0.0927(2) 0.0237(7) Uani 1.00 d
S(3) S 0.3052(2) 0.1435(1) 0.2983(2) 0.0259(7) Uani 1.00 d
S(4) S -0.1844(2) 0.0587(1) 0.0597(2) 0.0257(7) Uani 1.00 d
P(1) P 0.1610(2) 0.1442(1) -0.0172(2) 0.0218(7) Uani 1.00 d
P(2) P 0.3125(2) 0.0989(1) 0.4096(2) 0.0211(6) Uani 1.00 d
O(1) O 0.0071(5) 0.0242(2) 0.1588(4) 0.018(2) Uani 1.00 d
O(2) O 0.1714(5) 0.0476(2) 0.1984(4) 0.018(2) Uani 1.00 d
O(3) O -0.0641(5) 0.1785(3) 0.1066(4) 0.020(2) Uani 1.00 d
O(4) O 0.1098(5) 0.2010(3) 0.2522(4) 0.021(2) Uani 1.00 d
O(5) O 0.1148(6) 0.2001(3) -0.0484(5) 0.032(2) Uani 1.00 d
O(6) O 0.2356(5) 0.1296(3) -0.0994(4) 0.024(2) Uani 1.00 d
O(7) O 0.4048(5) 0.0576(3) 0.4053(4) 0.025(2) Uani 1.00 d
O(8) O 0.3515(5) 0.1361(3) 0.4908(5) 0.031(2) Uani 1.00 d
C(1) C 0.1003(7) 0.0133(4) 0.1804(6) 0.018(2) Uani 1.00 d
C(2) C 0.1294(8) -0.0447(4) 0.1861(7) 0.028(3) Uani 1.00 d
C(3) C -0.0894(7) 0.2123(4) 0.1663(6) 0.021(3) Uani 1.00 d
C(4) C -0.0964(10) 0.2702(4) 0.1384(7) 0.037(3) Uani 1.00 d
C(5) C 0.049(1) 0.2036(6) -0.1292(8) 0.061(5) Uani 1.00 d
C(6) C -0.0181(9) 0.2527(5) -0.1191(8) 0.044(4) Uani 1.00 d
C(7) C 0.2874(8) 0.0776(4) -0.1022(7) 0.028(3) Uani 1.00 d
C(8) C 0.3812(9) 0.0821(5) -0.1626(8) 0.044(4) Uani 1.00 d
C(9) C 0.5132(8) 0.0762(5) 0.3915(8) 0.035(3) Uani 1.00 d
C(10) C 0.5802(8) 0.0275(5) 0.3768(8) 0.040(3) Uani 1.00 d
C(11) C 0.284(1) 0.1786(5) 0.5259(8) 0.044(4) Uani 1.00 d
C(12) C 0.297(1) 0.1822(6) 0.6242(8) 0.057(5) Uani 1.00 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.703 8.390
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 -3 -1
1 -3 1
1 -5 0
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pt(2) Pt(1) Pt(2) 88.79(4) 1_555 1_555 4_555 yes
Pt(2) Pt(1) S(1) 95.17(7) 1_555 1_555 1_555 yes
Pt(2) Pt(1) S(4) 166.95(7) 1_555 1_555 1_555 yes
Pt(2) Pt(1) O(1) 84.9(2) 1_555 1_555 1_555 yes
Pt(2) Pt(1) O(3) 93.9(2) 1_555 1_555 1_555 yes
Pt(2) Pt(1) S(1) 173.97(7) 4_555 1_555 1_555 yes
Pt(2) Pt(1) S(4) 93.79(7) 4_555 1_555 1_555 yes
Pt(2) Pt(1) O(1) 101.2(2) 4_555 1_555 1_555 yes
Pt(2) Pt(1) O(3) 82.4(2) 4_555 1_555 1_555 yes
S(1) Pt(1) S(4) 83.36(9) 1_555 1_555 1_555 yes
S(1) Pt(1) O(1) 83.7(2) 1_555 1_555 1_555 yes
S(1) Pt(1) O(3) 92.8(2) 1_555 1_555 1_555 yes
S(4) Pt(1) O(1) 82.0(2) 1_555 1_555 1_555 yes
S(4) Pt(1) O(3) 99.1(2) 1_555 1_555 1_555 yes
O(1) Pt(1) O(3) 176.2(2) 1_555 1_555 1_555 yes
Pt(1) Pt(2) Pt(1) 85.82(3) 1_555 1_555 4_555 yes
Pt(1) Pt(2) S(2) 98.79(6) 1_555 1_555 1_555 yes
Pt(1) Pt(2) S(3) 177.39(6) 1_555 1_555 1_555 yes
Pt(1) Pt(2) O(2) 83.8(2) 1_555 1_555 1_555 yes
Pt(1) Pt(2) O(4) 100.1(2) 1_555 1_555 1_555 yes
Pt(1) Pt(2) S(2) 172.29(6) 4_555 1_555 1_555 yes
Pt(1) Pt(2) S(3) 96.12(7) 4_555 1_555 1_555 yes
Pt(1) Pt(2) O(2) 92.7(2) 4_555 1_555 1_555 yes
Pt(1) Pt(2) O(4) 85.8(2) 4_555 1_555 1_555 yes
S(2) Pt(2) S(3) 79.47(9) 1_555 1_555 1_555 yes
S(2) Pt(2) O(2) 94.0(2) 1_555 1_555 1_555 yes
S(2) Pt(2) O(4) 87.3(2) 1_555 1_555 1_555 yes
S(3) Pt(2) O(2) 94.4(2) 1_555 1_555 1_555 yes
S(3) Pt(2) O(4) 81.8(2) 1_555 1_555 1_555 yes
O(2) Pt(2) O(4) 175.7(3) 1_555 1_555 1_555 yes
Pt(1) S(1) P(1) 104.4(1) 1_555 1_555 1_555 yes
Pt(2) S(2) P(1) 106.5(1) 1_555 1_555 1_555 yes
Pt(2) S(3) P(2) 108.4(1) 1_555 1_555 1_555 yes
Pt(1) S(4) P(2) 108.8(1) 1_555 1_555 4_555 yes
S(1) P(1) S(2) 116.3(2) 1_555 1_555 1_555 yes
S(1) P(1) O(5) 113.5(3) 1_555 1_555 1_555 yes
S(1) P(1) O(6) 107.0(3) 1_555 1_555 1_555 yes
S(2) P(1) O(5) 107.0(3) 1_555 1_555 1_555 yes
S(2) P(1) O(6) 110.7(3) 1_555 1_555 1_555 yes
O(5) P(1) O(6) 101.4(4) 1_555 1_555 1_555 yes
S(3) P(2) S(4) 115.9(2) 1_555 1_555 4_555 yes
S(3) P(2) O(7) 111.5(3) 1_555 1_555 1_555 yes
S(3) P(2) O(8) 108.5(3) 1_555 1_555 1_555 yes
S(4) P(2) O(7) 107.4(3) 4_555 1_555 1_555 yes
S(4) P(2) O(8) 112.1(3) 4_555 1_555 1_555 yes
O(7) P(2) O(8) 100.2(4) 1_555 1_555 1_555 yes
Pt(1) O(1) C(1) 119.1(6) 1_555 1_555 1_555 yes
Pt(2) O(2) C(1) 121.6(6) 1_555 1_555 1_555 yes
Pt(1) O(3) C(3) 122.4(6) 1_555 1_555 1_555 yes
Pt(2) O(4) C(3) 117.9(6) 1_555 1_555 4_555 yes
P(1) O(5) C(5) 120.3(7) 1_555 1_555 1_555 yes
P(1) O(6) C(7) 119.7(6) 1_555 1_555 1_555 yes
P(2) O(7) C(9) 120.4(7) 1_555 1_555 1_555 yes
P(2) O(8) C(11) 120.4(7) 1_555 1_555 1_555 yes
O(1) C(1) O(2) 125.4(9) 1_555 1_555 1_555 yes
O(1) C(1) C(2) 117.2(8) 1_555 1_555 1_555 yes
O(2) C(1) C(2) 117.3(8) 1_555 1_555 1_555 yes
O(3) C(3) O(4) 125.0(9) 1_555 1_555 4_555 yes
O(3) C(3) C(4) 117.4(9) 1_555 1_555 1_555 yes
O(4) C(3) C(4) 117.6(9) 4_555 1_555 1_555 yes
O(5) C(5) C(6) 106.9(10) 1_555 1_555 1_555 yes
O(6) C(7) C(8) 108.2(8) 1_555 1_555 1_555 yes
O(7) C(9) C(10) 107.5(9) 1_555 1_555 1_555 yes
O(8) C(11) C(12) 109.4(10) 1_555 1_555 1_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt(1) Pt(2) 2.583(1) 1_555 1_555 yes
Pt(1) Pt(2) 2.5836(7) 1_555 4_555 yes
Pt(1) S(1) 2.461(3) 1_555 1_555 yes
Pt(1) S(4) 2.492(3) 1_555 1_555 yes
Pt(1) O(1) 2.033(6) 1_555 1_555 yes
Pt(1) O(3) 2.006(6) 1_555 1_555 yes
Pt(2) S(2) 2.500(3) 1_555 1_555 yes
Pt(2) S(3) 2.485(3) 1_555 1_555 yes
Pt(2) O(2) 1.994(6) 1_555 1_555 yes
Pt(2) O(4) 2.004(6) 1_555 1_555 yes
S(1) P(1) 1.991(4) 1_555 1_555 yes
S(2) P(1) 1.983(4) 1_555 1_555 yes
S(3) P(2) 2.003(4) 1_555 1_555 yes
S(4) P(2) 1.975(4) 1_555 4_555 yes
P(1) O(5) 1.589(7) 1_555 1_555 yes
P(1) O(6) 1.597(7) 1_555 1_555 yes
P(2) O(7) 1.570(7) 1_555 1_555 yes
P(2) O(8) 1.607(7) 1_555 1_555 yes
O(1) C(1) 1.26(1) 1_555 1_555 yes
O(2) C(1) 1.28(1) 1_555 1_555 yes
O(3) C(3) 1.27(1) 1_555 1_555 yes
O(4) C(3) 1.28(1) 1_555 4_555 yes
O(5) C(5) 1.48(1) 1_555 1_555 yes
O(6) C(7) 1.46(1) 1_555 1_555 yes
O(7) C(9) 1.48(1) 1_555 1_555 yes
O(8) C(11) 1.47(1) 1_555 1_555 yes
C(1) C(2) 1.50(1) 1_555 1_555 yes
C(3) C(4) 1.51(1) 1_555 1_555 yes
C(5) C(6) 1.50(2) 1_555 1_555 yes
C(7) C(8) 1.51(1) 1_555 1_555 yes
C(9) C(10) 1.50(1) 1_555 1_555 yes
C(11) C(12) 1.48(1) 1_555 1_555 yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
S(1) S(4) 3.293(4) 1_555 1_555
S(1) S(2) 3.375(4) 1_555 1_555
S(2) S(3) 3.187(4) 1_555 1_555
S(3) S(4) 3.372(4) 1_555 4_555
