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#$Date: 2016-03-23 15:25:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179327 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/24/4322409.cif $
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#
# 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_4322409
loop_
_publ_author_name
'Christopher E. Keefer'
'Suzanne T. Purrington'
'Robert D. Bereman'
'Paul D. Boyle'
_publ_contact_author
;
Professor Robert D. Bereman
Department of Chemistry
Box 8204
North Carolina State University
Raleigh, NC 27695-8204
USA
;
_publ_contact_author_email       R_Bereman@ncsu.edu
_publ_contact_author_fax         1(919)5155079
_publ_contact_author_phone       1(919)5151963
_publ_section_title
;
 The First Systematic Synthesis of Heterobimetallic Dithiolene-Bridged
 Complexes. Synthesis and Characterization of Metal Complexes of
 4-(1',2'-Ethylenedithiolate)-1,3-dithiole-2-one and Dimeric Metal
 Complexes of 1,2,3,4-Butadienetetrathiolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5437
_journal_page_last               5442
_journal_paper_doi               10.1021/ic990841a
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C16 H15 O2 Pt S6'
_chemical_formula_sum            'C16 H15 O2 Pt S6'
_chemical_formula_weight         626.74
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 97.289(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.0388(4)
_cell_length_b                   9.2048(3)
_cell_length_c                   16.2384(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      19.50
_cell_volume                     1933.18(11)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Theta/2theta scan b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5590
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.97
_exptl_absorpt_correction_T_max  .9993
_exptl_absorpt_correction_T_min  .4656
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_description       needle
_exptl_crystal_F_000             1199.29
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .04
_refine_diff_density_max         1.99
_refine_diff_density_min         -1.03
_refine_ls_extinction_coef       0.0074(12)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   1.48
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4394
_refine_ls_R_factor_all          .035
_refine_ls_R_factor_obs          .035
_refine_ls_shift/esd_max         .049
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .047
_refine_ls_wR_factor_obs         .046
_reflns_number_observed          4396
_reflns_number_total             5590
_reflns_observed_criterion       'Inet > 1.5\s(Inet)'
_cod_data_source_file            ic990841a_2.cif
_cod_data_source_block           2^.^(1/2)1
_cod_original_cell_volume        1933.18(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4322409
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Pt .771895(15) .162751(20) .344197(12) .03209(10) Uij ? . Pt
S1 .65005(12) .24746(16) .24324(10) .0441(7) Uij ? . S
S2 .64934(10) .01882(16) .39024(9) .0394(6) Uij ? . S
S3 .33635(12) -.01661(20) .25678(12) .0572(9) Uij ? . S
S4 .32327(15) -.2227(3) .39227(13) .0679(11) Uij ? . S
O1 .1662(4) -.1569(5) .2791(4) .070(3) Uij ? . O
C1 .5397(4) .1512(6) .2586(4) .039(3) Uij ? . C
C2 .5391(4) .0533(6) .3193(4) .038(3) Uij ? . C
C3 .4466(4) -.0346(6) .3309(4) .041(3) Uij ? . C
C4 .4385(5) -.1298(8) .3913(4) .052(3) Uij ? . C
C5 .2572(5) -.1349(7) .3047(5) .053(4) Uij ? . C
C6 .8691(5) .1415(6) .4646(3) .041(3) Uij ? . C
C7 .9038(4) .0418(6) .4114(4) .041(3) Uij ? . C
C8 1.0032(5) .0590(7) .3695(4) .045(3) Uij ? . C
C9 .9812(5) .1256(7) .2840(4) .050(3) Uij ? . C
C10 .8952(5) .2356(7) .2727(4) .044(3) Uij ? . C
C11 .8795(5) .3440(6) .3309(4) .045(3) Uij ? . C
C12 .9484(6) .3740(7) .4106(5) .056(4) Uij ? . C
C13 .9174(5) .2891(8) .4862(4) .053(3) Uij ? . C
S5 .85635(20) .0310(3) .05561(14) .0820(14) Uij ? . S
S6 .82195(24) .2364(4) -.08408(17) .0989(19) Uij ? . S
O2 .6875(6) .1922(9) .0202(6) .114(6) Uij ? . O
C14 .9538(5) .0442(8) -.0079(4) .056(4) Uij ? . C
C15 .9254(8) .1457(8) -.0696(5) .074(5) Uij ? . C
C16 .7716(7) .1554(11) .0042(8) .099(7) Uij ? . C
H1 .479 .170 .220 .0488 Uiso ? . H
H4 .496 -.146 .434 .0624 Uiso ? . H
H6 .825 .107 .503 .0504 Uiso ? . H
H7 .881 -.057 .415 .0498 Uiso ? . H
H8a 1.036 -.033 .365 .0552 Uiso ? . H
H8b 1.050 .122 .403 .0552 Uiso ? . H
H9a 1.043 .171 .270 .0600 Uiso ? . H
H9b .964 .048 .245 .0600 Uiso ? . H
H10 .864 .250 .217 .0535 Uiso ? . H
H11 .838 .425 .310 .0544 Uiso ? . H
H12a 1.018 .347 .402 .0651 Uiso ? . H
H12b .949 .477 .421 .0651 Uiso ? . H
H13a .869 .348 .511 .0621 Uiso ? . H
H13b .978 .275 .526 .0621 Uiso ? . H
H15 .974 .163 -.108 .0821 Uiso ? . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt ? -2.352 8.388 'International Tables Vol. IV Table 2.2B'
S ? .110 .124 'International Tables Vol. IV Table 2.2B'
O ? .008 .006 'International Tables Vol. IV Table 2.2B'
C ? .002 .002 'International Tables Vol. IV Table 2.2B'
H ? .000 .000 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
8 2 3
2 5 2
2 2 -11
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
S1 Pt S2 88.91(5) ? ? ? ?
S1 Pt C6 160.65(16) ? ? ? ?
S1 Pt C7 162.90(16) ? ? ? ?
S1 Pt C10 90.31(16) ? ? ? ?
S1 Pt C11 93.75(17) ? ? ? ?
S2 Pt C6 90.33(15) ? ? ? ?
S2 Pt C7 94.56(15) ? ? ? ?
S2 Pt C10 160.15(18) ? ? ? ?
S2 Pt C11 162.57(18) ? ? ? ?
C6 Pt C7 36.32(22) ? ? ? ?
C6 Pt C10 96.82(22) ? ? ? ?
C6 Pt C11 81.49(22) ? ? ? ?
C7 Pt C10 80.78(22) ? ? ? ?
C7 Pt C11 87.96(21) ? ? ? ?
C10 Pt C11 37.21(24) ? ? ? ?
Pt S1 C1 103.75(20) ? ? ? ?
Pt S2 C2 103.31(19) ? ? ? ?
C3 S3 C5 96.6(3) ? ? ? ?
C4 S4 C5 95.9(3) ? ? ? ?
S1 C1 C2 122.2(4) ? ? ? ?
S2 C2 C1 121.7(4) ? ? ? ?
S2 C2 C3 115.5(4) ? ? ? ?
C1 C2 C3 122.8(5) ? ? ? ?
S3 C3 C2 117.9(4) ? ? ? ?
S3 C3 C4 115.6(5) ? ? ? ?
C2 C3 C4 126.5(6) ? ? ? ?
S4 C4 C3 118.9(5) ? ? ? ?
S3 C5 S4 112.8(4) ? ? ? ?
S3 C5 O1 123.6(7) ? ? ? ?
S4 C5 O1 123.5(6) ? ? ? ?
Pt C6 C7 72.5(3) ? ? ? ?
Pt C6 C13 107.5(4) ? ? ? ?
C7 C6 C13 125.6(5) ? ? ? ?
Pt C7 C6 71.2(3) ? ? ? ?
Pt C7 C8 111.9(4) ? ? ? ?
C6 C7 C8 124.7(5) ? ? ? ?
C7 C8 C9 111.9(5) ? ? ? ?
C8 C9 C10 115.9(5) ? ? ? ?
Pt C10 C9 108.2(4) ? ? ? ?
Pt C10 C11 71.6(3) ? ? ? ?
C9 C10 C11 124.3(6) ? ? ? ?
Pt C11 C10 71.2(3) ? ? ? ?
Pt C11 C12 111.9(4) ? ? ? ?
C10 C11 C12 125.9(6) ? ? ? ?
C11 C12 C13 113.7(5) ? ? ? ?
C6 C13 C12 114.2(5) ? ? ? ?
C14 S5 C16 97.9(5) ? ? ? ?
C15 S6 C16 93.0(4) ? ? ? ?
S5 C14 C14a 120.6(5) ? ? ? ?
S5 C14 C15 109.1(6) ? ? ? ?
C14a C14 C15 130.3(7) ? ? ? ?
S6 C15 C14 127.6(7) ? ? ? ?
S5 C16 S6 112.4(5) ? ? ? ?
S5 C16 O2 128.6(11) ? ? ? ?
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 S1 2.2713(15) ? ? ?
Pt S2 2.2740(13) ? ? ?
Pt C6 2.200(6) ? ? ?
Pt C7 2.216(6) ? ? ?
Pt C10 2.203(5) ? ? ?
Pt C11 2.208(5) ? ? ?
S1 C1 1.734(6) ? ? ?
S2 C2 1.752(6) ? ? ?
S3 C3 1.761(6) ? ? ?
S3 C5 1.749(7) ? ? ?
S4 C4 1.731(7) ? ? ?
S4 C5 1.763(9) ? ? ?
O1 C5 1.222(9) ? ? ?
C1 C2 1.336(8) ? ? ?
C2 C3 1.485(8) ? ? ?
C3 C4 1.329(9) ? ? ?
C6 C7 1.376(8) ? ? ?
C6 C13 1.520(9) ? ? ?
C7 C8 1.546(8) ? ? ?
C8 C9 1.510(9) ? ? ?
C9 C10 1.505(9) ? ? ?
C10 C11 1.407(9) ? ? ?
C11 C12 1.504(10) ? ? ?
C12 C13 1.550(10) ? ? ?
S5 C14 1.740(7) ? ? ?
S5 C16 1.731(12) ? ? ?
S6 C15 1.579(11) ? ? ?
S6 C16 1.811(14) ? ? ?
O2 C16 1.207(13) ? ? ?
C14 C14a 1.450(15) ? ? ?
