#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/52/7025258.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_7025258
loop_
_publ_author_name
'Djinovic, Vesna M.'
'Galanski, Markus'
'Arion, Vladimir B.'
'Keppler, Bernhard K.'
_publ_section_title
;
 Synthesis and structures of novel 1-methylcytosinato-bridged
 (ethylenediamine)platinum(II) and platinum(III) dinuclear complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3633
_journal_page_last               3643
_journal_paper_doi               10.1039/b926133h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C14 H28 N10 O10 Pt2 S2, 2(H2 O), 2(O0.80)'
_chemical_formula_sum            'C14 H35.2 N10 O13.6 Pt2 S2'
_chemical_formula_weight         1015.62
_chemical_name_common
;
Bis(ethane-1,2-diamine-1kappa$2!N,N',2kappa$2!N,N')bis(miu-1-
methylcytosinato-kappa$2!N3,N4)(disulfato-
1kappaO,2kappaO)diplatinum(iii)(Pt-Pt) hydrate
;
_chemical_name_systematic
;
Bis(ethane-1,2-diamine-1kappa²N,N',2kappa²N,N')bis(miu-1-methylcytosinato-
kappa²N3,N4)(disulfato-1kappaO,2kappaO)diplatinum(III)(Pt-Pt) hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 125.859(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8579(6)
_cell_length_b                   12.0130(6)
_cell_length_c                   14.3117(6)
_cell_measurement_reflns_used    489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.38
_cell_volume                     2767.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23112
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    10.334
_exptl_absorpt_correction_T_max  0.8200
_exptl_absorpt_correction_T_min  0.4247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0270
_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)+(0.0313P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                2191
_reflns_number_total             2718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926133h.txt
_cod_data_source_block           vedj047
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C14 H35.20 N10 O13.60 Pt2 S2'
_cod_database_code               7025258
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
Pt1A Pt 0.058173(13) 0.290819(19) 0.234354(19) 0.00843(8) Uani 1 1 d .
S1A S 0.23633(9) 0.20164(14) 0.29653(13) 0.0144(3) Uani 1 1 d .
O1A O 0.1522(2) 0.2583(3) 0.2089(4) 0.0119(9) Uani 1 1 d .
O2A O 0.2823(3) 0.2088(4) 0.2473(4) 0.0242(11) Uani 1 1 d .
O3A O 0.2196(2) 0.0838(3) 0.3076(4) 0.0185(10) Uani 1 1 d .
O4A O 0.2771(2) 0.2562(4) 0.4077(4) 0.0173(10) Uani 1 1 d .
N1A N -0.0663(3) 0.1200(5) -0.0858(4) 0.0172(12) Uani 1 1 d .
C2A C -0.0255(3) 0.2054(5) -0.0060(5) 0.0129(12) Uani 1 1 d .
N3A N -0.0254(3) 0.2018(4) 0.0902(4) 0.0112(10) Uani 1 1 d .
C4A C -0.0773(3) 0.1297(5) 0.0959(5) 0.0116(12) Uani 1 1 d .
C5A C -0.1117(3) 0.0390(5) 0.0179(5) 0.0142(13) Uani 1 1 d .
H5 H -0.1385 -0.0202 0.0284 0.017 Uiso 1 1 calc R
C6A C -0.1060(4) 0.0380(5) -0.0702(5) 0.0165(14) Uani 1 1 d .
H6 H -0.1304 -0.0218 -0.1237 0.020 Uiso 1 1 calc R
C7A C -0.0702(4) 0.1261(6) -0.1906(5) 0.0246(16) Uani 1 1 d .
H7A H -0.1104 0.0714 -0.2465 0.037 Uiso 1 1 calc R
H7B H -0.0152 0.1099 -0.1721 0.037 Uiso 1 1 calc R
H7C H -0.0876 0.2010 -0.2235 0.037 Uiso 1 1 calc R
O8A O 0.0081(3) 0.2814(4) -0.0226(4) 0.0188(10) Uani 1 1 d .
N9A N -0.0895(3) 0.1501(4) 0.1739(4) 0.0108(11) Uani 1 1 d .
H90 H -0.1215 0.1103 0.1712 0.013 Uiso 1 1 d R
N10A N 0.0405(3) 0.4375(4) 0.1487(4) 0.0104(11) Uani 1 1 d .
H10A H 0.0575 0.4289 0.1016 0.013 Uiso 1 1 calc R
H10B H -0.0152 0.4550 0.1031 0.013 Uiso 1 1 calc R
N11A N 0.1460(3) 0.3814(4) 0.3756(4) 0.0115(11) Uani 1 1 d .
H11A H 0.1257 0.4030 0.4165 0.014 Uiso 1 1 calc R
H11B H 0.1927 0.3388 0.4231 0.014 Uiso 1 1 calc R
C10A C 0.0883(4) 0.5305(5) 0.2319(5) 0.0159(14) Uani 1 1 d .
H10C H 0.0550 0.5653 0.2551 0.019 Uiso 1 1 calc R
H10D H 0.1017 0.5881 0.1957 0.019 Uiso 1 1 calc R
C11A C 0.1672(3) 0.4817(5) 0.3358(5) 0.0139(13) Uani 1 1 d .
H11C H 0.2053 0.4604 0.3153 0.017 Uiso 1 1 calc R
H11D H 0.1956 0.5376 0.3984 0.017 Uiso 1 1 calc R
O5 O 0.3709(2) 0.9845(4) 0.4659(3) 0.0169(10) Uani 1 1 d .
H5E H 0.3239 1.0158 0.4164 0.020 Uiso 1 1 d R
H5F H 0.3620 0.9172 0.4763 0.020 Uiso 1 1 d R
O6 O 0.3397(10) 0.762(2) 0.498(2) 0.022(4) Uani 0.50 1 d P
O6X O 0.307(2) 0.763(4) 0.476(4) 0.056(12) Uani 0.30 1 d P
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'
S S 0.1246 0.1234 '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
N9A Pt1A N3A 88.7(2) 2 .
N9A Pt1A N11A 92.49(19) 2 .
N3A Pt1A N11A 176.80(18) . .
N9A Pt1A N10A 173.30(18) 2 .
N3A Pt1A N10A 95.32(19) . .
N11A Pt1A N10A 83.23(19) . .
N9A Pt1A O1A 89.45(17) 2 .
N3A Pt1A O1A 90.37(17) . .
N11A Pt1A O1A 86.66(17) . .
N10A Pt1A O1A 85.17(17) . .
N9A Pt1A Pt1A 81.58(13) 2 2
N3A Pt1A Pt1A 83.99(13) . 2
N11A Pt1A Pt1A 99.13(13) . 2
N10A Pt1A Pt1A 104.14(13) . 2
O1A Pt1A Pt1A 169.49(11) . 2
O2A S1A O4A 113.6(3) . .
O2A S1A O3A 110.7(3) . .
O4A S1A O3A 109.3(3) . .
O2A S1A O1A 105.7(2) . .
O4A S1A O1A 109.6(2) . .
O3A S1A O1A 107.8(2) . .
S1A O1A Pt1A 125.5(2) . .
C6A N1A C2A 121.0(5) . .
C6A N1A C7A 121.3(5) . .
C2A N1A C7A 117.5(5) . .
O8A C2A N3A 122.1(6) . .
O8A C2A N1A 120.6(5) . .
N3A C2A N1A 117.2(6) . .
C2A N3A C4A 120.9(5) . .
C2A N3A Pt1A 121.3(4) . .
C4A N3A Pt1A 117.5(4) . .
N9A C4A N3A 116.9(5) . .
N9A C4A C5A 125.2(6) . .
N3A C4A C5A 117.9(5) . .
C6A C5A C4A 118.9(6) . .
C6A C5A H5 120.5 . .
C4A C5A H5 120.5 . .
C5A C6A N1A 121.9(6) . .
C5A C6A H6 119.0 . .
N1A C6A H6 119.0 . .
N1A C7A H7A 109.5 . .
N1A C7A H7B 109.5 . .
H7A C7A H7B 109.5 . .
N1A C7A H7C 109.5 . .
H7A C7A H7C 109.5 . .
H7B C7A H7C 109.5 . .
C4A N9A Pt1A 125.5(4) . 2
C4A N9A H90 113.5 . .
Pt1A N9A H90 118.9 2 .
C10A N10A Pt1A 111.0(3) . .
C10A N10A H10A 109.4 . .
Pt1A N10A H10A 109.4 . .
C10A N10A H10B 109.4 . .
Pt1A N10A H10B 109.4 . .
H10A N10A H10B 108.0 . .
C11A N11A Pt1A 108.6(3) . .
C11A N11A H11A 110.0 . .
Pt1A N11A H11A 110.0 . .
C11A N11A H11B 110.0 . .
Pt1A N11A H11B 110.0 . .
H11A N11A H11B 108.3 . .
N10A C10A C11A 107.6(5) . .
N10A C10A H10C 110.2 . .
C11A C10A H10C 110.2 . .
N10A C10A H10D 110.2 . .
C11A C10A H10D 110.2 . .
H10C C10A H10D 108.5 . .
N11A C11A C10A 109.0(5) . .
N11A C11A H11C 109.9 . .
C10A C11A H11C 109.9 . .
N11A C11A H11D 109.9 . .
C10A C11A H11D 109.9 . .
H11C C11A H11D 108.3 . .
H5E O5 H5F 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1A N9A 2.002(5) 2
Pt1A N3A 2.035(5) .
Pt1A N11A 2.045(5) .
Pt1A N10A 2.056(5) .
Pt1A O1A 2.138(4) .
Pt1A Pt1A 2.5982(4) 2
S1A O2A 1.446(4) .
S1A O4A 1.451(4) .
S1A O3A 1.483(4) .
S1A O1A 1.540(4) .
N1A C6A 1.360(8) .
N1A C2A 1.390(8) .
N1A C7A 1.457(8) .
C2A O8A 1.233(7) .
C2A N3A 1.377(7) .
N3A C4A 1.386(7) .
C4A N9A 1.297(7) .
C4A C5A 1.416(8) .
C5A C6A 1.331(8) .
C5A H5 0.9500 .
C6A H6 0.9500 .
C7A H7A 0.9800 .
C7A H7B 0.9800 .
C7A H7C 0.9800 .
N9A Pt1A 2.002(5) 2
N9A H90 0.7782 .
N10A C10A 1.497(7) .
N10A H10A 0.9200 .
N10A H10B 0.9200 .
N11A C11A 1.495(7) .
N11A H11A 0.9200 .
N11A H11B 0.9200 .
C10A C11A 1.510(8) .
C10A H10C 0.9900 .
C10A H10D 0.9900 .
C11A H11C 0.9900 .
C11A H11D 0.9900 .
O5 H5E 0.8607 .
O5 H5F 0.8597 .
O6 O6X 0.52(4) .
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
_geom_torsion_site_symmetry_4
O2A S1A O1A Pt1A -173.9(3) . .
O4A S1A O1A Pt1A -51.1(4) . .
O3A S1A O1A Pt1A 67.7(3) . .
N9A Pt1A O1A S1A -34.1(3) 2 .
N3A Pt1A O1A S1A -122.8(3) . .
N11A Pt1A O1A S1A 58.4(3) . .
N10A Pt1A O1A S1A 141.9(3) . .
Pt1A Pt1A O1A S1A -65.4(7) 2 .
C6A N1A C2A O8A -177.6(5) . .
C7A N1A C2A O8A -2.0(8) . .
C6A N1A C2A N3A 1.5(8) . .
C7A N1A C2A N3A 177.0(5) . .
O8A C2A N3A C4A 166.5(5) . .
N1A C2A N3A C4A -12.6(8) . .
O8A C2A N3A Pt1A -19.5(8) . .
N1A C2A N3A Pt1A 161.5(4) . .
N9A Pt1A N3A C2A -126.8(5) 2 .
N10A Pt1A N3A C2A 47.8(5) . .
O1A Pt1A N3A C2A -37.4(5) . .
Pt1A Pt1A N3A C2A 151.5(4) 2 .
N9A Pt1A N3A C4A 47.5(4) 2 .
N10A Pt1A N3A C4A -137.9(4) . .
O1A Pt1A N3A C4A 136.9(4) . .
Pt1A Pt1A N3A C4A -34.2(4) 2 .
C2A N3A C4A N9A -162.9(5) . .
Pt1A N3A C4A N9A 22.8(7) . .
C2A N3A C4A C5A 18.1(8) . .
Pt1A N3A C4A C5A -156.2(4) . .
N9A C4A C5A C6A 168.6(6) . .
N3A C4A C5A C6A -12.5(8) . .
C4A C5A C6A N1A 1.7(9) . .
C2A N1A C6A C5A 3.9(9) . .
C7A N1A C6A C5A -171.5(6) . .
N3A C4A N9A Pt1A 12.4(7) . 2
C5A C4A N9A Pt1A -168.7(4) . 2
N3A Pt1A N10A C10A 174.4(4) . .
N11A Pt1A N10A C10A -8.4(4) . .
O1A Pt1A N10A C10A -95.6(4) . .
Pt1A Pt1A N10A C10A 89.3(3) 2 .
N9A Pt1A N11A C11A 156.3(4) 2 .
N10A Pt1A N11A C11A -18.5(4) . .
O1A Pt1A N11A C11A 67.0(3) . .
Pt1A Pt1A N11A C11A -121.8(3) 2 .
Pt1A N10A C10A C11A 33.2(5) . .
Pt1A N11A C11A C10A 42.3(5) . .
N10A C10A C11A N11A -49.5(6) . .
