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#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327434.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_4327434
loop_
_publ_author_name
'Takashi Kubo'
'Misako Ohsahi'
'Katsuaki Miyazaki'
'Akio Ichimura'
'Kazuhiro Nakasuji'
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, Osaka University 
Machikaneyama 1-1, Toyonaka, Osaka, 560-0043, Japan
;
_publ_contact_author_email       kubo@chem.sci.osaka-u.ac.jp
_publ_contact_author_fax         '+81 6 6850 5395'
_publ_contact_author_name        'Takashi Kubo'
_publ_contact_author_phone       '+81 6 6850 5394'
_publ_section_title
;
 Synthesis, Structure, and Cooperative Proton-Electron Transfer Reaction
 of Bis(5,6-diethylpyrazinedithiolato)metal Complexes (M = Ni, Pd, Pt)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7301
_journal_page_last               7307
_journal_paper_doi               10.1021/ic049621+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24 H40 N6 O2 Pt S4'
_chemical_formula_weight         767.95
_chemical_name_common            Pt(Hdepdt)2-DMAC
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 97.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.905(15)
_cell_length_b                   12.227(9)
_cell_length_c                   15.752(14)
_cell_measurement_reflns_used    12581
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     3040(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3475
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0374
_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)+(0.0130P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                2485
_reflns_number_total             3475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0496212Bsi20040322_012110_4.cif
_cod_data_source_block           PtDMAC
_cod_database_code               4327434
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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 0.23850(2) -0.2500 0.03116(10) Uani 1 2 d S
S1 S 0.95023(10) 0.10617(10) -0.34768(8) 0.0388(4) Uani 1 1 d .
S2 S 0.95120(10) 0.37073(10) -0.34613(8) 0.0368(4) Uani 1 1 d .
O1 O 0.8478(3) -0.0919(3) -0.5162(3) 0.0737(15) Uani 1 1 d .
N1 N 0.8639(3) 0.1315(3) -0.5014(3) 0.0326(11) Uani 1 1 d .
N2 N 0.8686(3) 0.3526(3) -0.5009(2) 0.0346(11) Uani 1 1 d .
N3 N 0.8833(5) -0.2627(5) -0.4927(6) 0.135(4) Uani 1 1 d .
C1 C 0.9039(3) 0.1814(4) -0.4319(3) 0.0292(12) Uani 1 1 d .
C2 C 0.9043(3) 0.2977(4) -0.4336(3) 0.0300(12) Uani 1 1 d .
C3 C 0.8293(3) 0.2983(4) -0.5699(3) 0.0316(12) Uani 1 1 d .
C4 C 0.8254(3) 0.1864(4) -0.5718(3) 0.0308(12) Uani 1 1 d .
C5 C 0.7934(4) 0.3697(4) -0.6442(3) 0.0422(16) Uani 1 1 d .
C6 C 0.7852(4) 0.1157(4) -0.6434(3) 0.0395(15) Uani 1 1 d .
C7 C 0.8616(5) 0.4077(5) -0.6971(4) 0.065(2) Uani 1 1 d .
C8 C 0.8481(4) 0.0753(5) -0.7012(4) 0.0584(19) Uani 1 1 d .
C9 C 0.8579(6) -0.1893(7) -0.5212(7) 0.117(4) Uani 1 1 d .
C10 C 0.9393(5) -0.2091(7) -0.4030(4) 0.092(3) Uani 1 1 d .
C11 C 0.8040(5) -0.2452(6) -0.6158(4) 0.078(2) Uani 1 1 d .
C12 C 0.8870(5) -0.3804(5) -0.4963(5) 0.081(3) Uani 1 1 d .
H1 H 0.8609 0.0523 -0.5022 0.046 Uiso 1 1 d .
H2 H 0.7592 0.0532 -0.6202 0.049 Uiso 1 1 d .
H3 H 0.7416 0.1558 -0.6775 0.049 Uiso 1 1 d .
H4 H 0.7516 0.3306 -0.6799 0.051 Uiso 1 1 d .
H5 H 0.7682 0.4332 -0.6223 0.051 Uiso 1 1 d .
H6 H 0.8909 0.0326 -0.6688 0.068 Uiso 1 1 d .
H7 H 0.8204 0.0307 -0.7462 0.068 Uiso 1 1 d .
H8 H 0.8738 0.1357 -0.7257 0.068 Uiso 1 1 d .
H9 H 0.8881 0.3447 -0.7197 0.075 Uiso 1 1 d .
H10 H 0.8388 0.4523 -0.7430 0.075 Uiso 1 1 d .
H11 H 0.9049 0.4471 -0.6619 0.075 Uiso 1 1 d .
H12 H 0.9695 -0.2584 -0.3678 0.109 Uiso 1 1 d .
H13 H 0.9810 -0.1530 -0.4200 0.109 Uiso 1 1 d .
H14 H 0.9031 -0.1651 -0.3703 0.109 Uiso 1 1 d .
H15 H 0.8315 -0.4127 -0.4948 0.100 Uiso 1 1 d .
H16 H 0.9067 -0.4053 -0.5487 0.100 Uiso 1 1 d .
H17 H 0.9239 -0.4097 -0.4497 0.100 Uiso 1 1 d .
H18 H 0.7759 -0.1914 -0.6519 0.096 Uiso 1 1 d .
H19 H 0.8437 -0.2830 -0.6488 0.096 Uiso 1 1 d .
H20 H 0.7630 -0.2998 -0.6040 0.096 Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S2 Pt1 S2 89.91(9) 2_754 .
S2 Pt1 S1 179.54(5) 2_754 .
S2 Pt1 S1 89.63(7) . .
S2 Pt1 S1 89.63(7) 2_754 2_754
S2 Pt1 S1 179.54(5) . 2_754
S1 Pt1 S1 90.83(9) . 2_754
C1 S1 Pt1 102.74(17) . .
C2 S2 Pt1 103.91(17) . .
C1 N1 C4 123.7(4) . .
C1 N1 H1 118.8(4) . .
C4 N1 H1 117.6(4) . .
C2 N2 C3 120.2(4) . .
C9 N3 C12 147.6(13) . .
C9 N3 C10 99.1(10) . .
C12 N3 C10 113.3(7) . .
N1 C1 C2 116.2(4) . .
N1 C1 S1 120.3(3) . .
C2 C1 S1 123.5(3) . .
N2 C2 C1 121.4(4) . .
N2 C2 S2 118.5(4) . .
C1 C2 S2 120.2(3) . .
N2 C3 C4 121.4(4) . .
N2 C3 C5 115.4(4) . .
C4 C3 C5 123.2(4) . .
C3 C4 N1 117.2(4) . .
C3 C4 C6 127.3(4) . .
N1 C4 C6 115.5(4) . .
C3 C5 C7 112.0(5) . .
C3 C5 H4 109.8(5) . .
C7 C5 H4 109.0(6) . .
C3 C5 H5 109.0(5) . .
C7 C5 H5 108.0(5) . .
H4 C5 H5 109.2(6) . .
C4 C6 C8 112.8(5) . .
C4 C6 H2 109.6(5) . .
C8 C6 H2 108.3(5) . .
C4 C6 H3 109.8(4) . .
C8 C6 H3 108.5(5) . .
H2 C6 H3 107.7(6) . .
C5 C7 H9 109.4(5) . .
C5 C7 H10 111.5(7) . .
H9 C7 H10 108.8(6) . .
C5 C7 H11 110.3(6) . .
H9 C7 H11 107.4(7) . .
H10 C7 H11 109.5(6) . .
C6 C8 H6 109.7(6) . .
C6 C8 H7 110.6(6) . .
H6 C8 H7 108.5(6) . .
C6 C8 H8 109.8(5) . .
H6 C8 H8 109.2(7) . .
H7 C8 H8 108.9(6) . .
N3 C9 O1 148.8(14) . .
N3 C9 C11 98.6(10) . .
O1 C9 C11 112.6(8) . .
N3 C10 H12 115.5(7) . .
N3 C10 H13 109.6(6) . .
H12 C10 H13 107.1(7) . .
N3 C10 H14 111.4(6) . .
H12 C10 H14 110.0(7) . .
H13 C10 H14 102.3(7) . .
C9 C11 H18 112.5(6) . .
C9 C11 H19 110.7(6) . .
H18 C11 H19 107.2(6) . .
C9 C11 H20 112.0(6) . .
H18 C11 H20 108.4(7) . .
H19 C11 H20 105.6(7) . .
N3 C12 H15 111.3(7) . .
N3 C12 H16 111.5(7) . .
H15 C12 H16 106.4(7) . .
N3 C12 H17 111.7(8) . .
H15 C12 H17 107.8(7) . .
H16 C12 H17 107.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 S2 2.2846(17) 2_754
Pt1 S2 2.2847(17) .
Pt1 S1 2.3047(18) .
Pt1 S1 2.3048(18) 2_754
S1 C1 1.705(5) .
S2 C2 1.731(5) .
O1 C9 1.205(9) .
N1 C1 1.344(5) .
N1 C4 1.374(5) .
N1 H1 0.970(4) .
N2 C2 1.322(5) .
N2 C3 1.359(5) .
N3 C9 1.061(9) .
N3 C12 1.442(8) .
N3 C10 1.706(11) .
C1 C2 1.423(6) .
C3 C4 1.369(6) .
C3 C5 1.513(6) .
C4 C6 1.500(6) .
C5 C7 1.519(9) .
C5 H4 0.946(5) .
C5 H5 0.957(6) .
C6 C8 1.516(9) .
C6 H2 0.963(5) .
C6 H3 0.958(5) .
C7 H9 0.966(7) .
C7 H10 0.941(5) .
C7 H11 0.959(6) .
C8 H6 0.954(6) .
C8 H7 0.957(5) .
C8 H8 0.949(7) .
C9 C11 1.763(12) .
C10 H12 0.915(7) .
C10 H13 1.012(9) .
C10 H14 0.979(8) .
C11 H18 0.946(7) .
C11 H19 0.981(7) .
C11 H20 0.966(7) .
C12 H15 0.969(8) .
C12 H16 0.968(8) .
C12 H17 0.951(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
S2 Pt1 S1 C1 7(8) 2_754
S2 Pt1 S1 C1 -1.81(19) .
S1 Pt1 S1 C1 178.3(2) 2_754
S2 Pt1 S2 C2 -178.8(2) 2_754
S1 Pt1 S2 C2 1.17(19) .
S1 Pt1 S2 C2 173(100) 2_754
C4 N1 C1 C2 0.6(8) .
C4 N1 C1 S1 -179.7(4) .
Pt1 S1 C1 N1 -177.3(4) .
Pt1 S1 C1 C2 2.5(5) .
C3 N2 C2 C1 0.9(8) .
C3 N2 C2 S2 -178.3(4) .
N1 C1 C2 N2 -1.3(8) .
S1 C1 C2 N2 179.0(4) .
N1 C1 C2 S2 178.0(4) .
S1 C1 C2 S2 -1.7(7) .
Pt1 S2 C2 N2 179.2(4) .
Pt1 S2 C2 C1 -0.1(5) .
C2 N2 C3 C4 0.1(8) .
C2 N2 C3 C5 -178.0(5) .
N2 C3 C4 N1 -0.8(9) .
C5 C3 C4 N1 177.2(5) .
N2 C3 C4 C6 -179.4(5) .
C5 C3 C4 C6 -1.4(10) .
C1 N1 C4 C3 0.5(8) .
C1 N1 C4 C6 179.2(5) .
N2 C3 C5 C7 79.0(6) .
C4 C3 C5 C7 -99.1(7) .
C3 C4 C6 C8 95.7(7) .
N1 C4 C6 C8 -82.9(6) .
C12 N3 C9 O1 169.4(12) .
C10 N3 C9 O1 -7(2) .
C12 N3 C9 C11 -6.1(18) .
C10 N3 C9 C11 177.6(5) .
