#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322345.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_4322345
loop_
_publ_author_name
'Richard A. Kortes'
'Steven J. Geib'
'Fu-Tyan Lin'
'Rex E. Shepherd'
_publ_section_title
;
 Crystal and Molecular Structure of a Potential DNA Groove-Spanning
 Chelate: [MV][Pt2(hdta)Cl2].4H2O (MV2+= 1,1'-Dimethyl-4,4'-bipyridinium,
 hdta4-= 1,6-Hexanediamine-N,N,N',N'-tetraacetate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5045
_journal_page_last               5052
_journal_paper_doi               10.1021/ic990123o
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C29 H20 Cl2 N2 O12 Pt2'
_chemical_formula_weight         1049.55
_chemical_name_systematic
;
 ?
;
_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                 109.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.757(5)
_cell_length_b                   13.566(3)
_cell_length_c                   12.120(2)
_cell_measurement_temperature    200(2)
_cell_volume                     3536.4(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3195
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    8.114
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_refine_diff_density_max         1.103
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0925P)²+18.8885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                2424
_reflns_number_total             3115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990123o.cif
_cod_data_source_block           sheperd
_cod_original_cell_volume        3536.4(12)
_cod_database_code               4322345
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt Pt 0.209866(17) -0.12131(2) 0.44507(3) 0.03820(17) Uani 1 1 d . . .
Cl Cl 0.14793(14) -0.1751(2) 0.2636(2) 0.0597(7) Uani 1 1 d . . .
O1 O 0.2849(3) -0.0953(5) 0.3963(6) 0.0462(16) Uani 1 1 d . . .
N1 N 0.2610(4) -0.0665(5) 0.5998(7) 0.047(2) Uani 1 1 d . . .
C1 C 0.3331(5) -0.0803(7) 0.4841(9) 0.048(2) Uani 1 1 d . . .
O2 O 0.1485(4) -0.1461(6) 0.5283(8) 0.064(2) Uani 1 1 d . . .
C2 C 0.3269(6) -0.0825(8) 0.6057(9) 0.053(3) Uani 1 1 d . . .
H2A H 0.3416 -0.1469 0.6428 0.063 Uiso 1 1 calc R . .
H2B H 0.3535 -0.0304 0.6545 0.063 Uiso 1 1 calc R . .
C3 C 0.2413(6) -0.1216(7) 0.6872(10) 0.051(3) Uani 1 1 d . . .
H3A H 0.2509 -0.0825 0.7599 0.061 Uiso 1 1 calc R . .
H3B H 0.2645 -0.1845 0.7059 0.061 Uiso 1 1 calc R . .
O3 O 0.3842(4) -0.0664(7) 0.4726(8) 0.073(3) Uani 1 1 d . . .
O4 O 0.1433(4) -0.1576(6) 0.7065(8) 0.071(2) Uani 1 1 d . . .
C4 C 0.1723(6) -0.1422(7) 0.6400(12) 0.054(3) Uani 1 1 d . . .
C5 C 0.2475(6) 0.0422(7) 0.6120(10) 0.057(3) Uani 1 1 d . . .
H5A H 0.2037 0.0490 0.6091 0.068 Uiso 1 1 calc R . .
H5B H 0.2742 0.0654 0.6896 0.068 Uiso 1 1 calc R . .
O5 O -0.0762(8) -0.0223(12) 0.7091(16) 0.068(4) Uani 0.50 1 d P . .
O6 O 0.0904(7) -0.3409(9) 0.7058(13) 0.127(5) Uani 1 1 d . . .
C6 C 0.2581(8) 0.1083(7) 0.5189(11) 0.066(4) Uani 1 1 d . . .
H6A H 0.2296 0.0893 0.4410 0.079 Uiso 1 1 calc R . .
H6B H 0.3013 0.1011 0.5188 0.079 Uiso 1 1 calc R . .
C7 C 0.2461(7) 0.2151(7) 0.5452(12) 0.069(4) Uani 1 1 d . . .
H7A H 0.2033 0.2209 0.5482 0.083 Uiso 1 1 calc R . .
H7B H 0.2753 0.2336 0.6228 0.083 Uiso 1 1 calc R . .
O7 O 0.0177(10) -0.4277(14) 0.7874(18) 0.084(6) Uani 0.50 1 d P . .
C11 C 0.0260(9) 0.0221(14) 0.4696(17) 0.042(4) Uani 0.50 1 d P . .
C12 C 0.0061(5) -0.0852(8) 0.4666(10) 0.051(3) Uani 1 1 d . . .
C13 C 0.0196(9) -0.1454(16) 0.373(2) 0.050(5) Uani 0.50 1 d P . .
C14 C 0.0023(10) -0.2425(13) 0.369(2) 0.049(5) Uani 0.50 1 d P . .
C15 C -0.0229(8) -0.2779(11) 0.4409(15) 0.032(4) Uani 0.50 1 d P . .
C16 C -0.0452(14) -0.3843(13) 0.429(2) 0.067(8) Uani 0.50 1 d P . .
C17 C -0.0769(13) -0.3257(15) 0.500(2) 0.066(7) Uani 0.50 1 d P . .
C18 C -0.0486(7) -0.2220(8) 0.5182(10) 0.063(3) Uani 1 1 d . . .
C19 C -0.0176(12) -0.1236(14) 0.536(2) 0.054(6) Uani 0.50 1 d P . .
C20 C -0.0852(9) -0.1572(16) 0.5677(18) 0.049(5) Uani 0.50 1 d P . .
C21 C -0.0701(10) -0.0589(16) 0.582(2) 0.050(5) Uani 0.50 1 d P . .
C22 C -0.0156(12) -0.1906(18) 0.469(2) 0.060(6) Uani 0.50 1 d P . .
C23 C 0.0096(9) -0.4007(14) 0.3396(18) 0.043(5) Uani 0.50 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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Pt O2 83.0(4) . . ?
N1 Pt O1 85.4(3) . . ?
O2 Pt O1 167.6(3) . . ?
N1 Pt Cl 176.5(2) . . ?
O2 Pt Cl 96.8(3) . . ?
O1 Pt Cl 95.0(2) . . ?
C1 O1 Pt 111.4(7) . . ?
C3 N1 C2 115.3(8) . . ?
C3 N1 C5 107.5(8) . . ?
C2 N1 C5 111.5(8) . . ?
C3 N1 Pt 105.3(6) . . ?
C2 N1 Pt 105.0(6) . . ?
C5 N1 Pt 112.1(7) . . ?
O3 C1 O1 121.3(11) . . ?
O3 C1 C2 120.0(10) . . ?
O1 C1 C2 118.6(10) . . ?
C4 O2 Pt 113.7(8) . . ?
N1 C2 C1 111.0(9) . . ?
N1 C3 C4 110.1(9) . . ?
O4 C4 O2 124.1(12) . . ?
O4 C4 C3 120.2(12) . . ?
O2 C4 C3 115.7(10) . . ?
C6 C5 N1 114.4(8) . . ?
C5 C6 C7 108.8(9) . . ?
C7 C7 C6 112.0(11) 7_556 . ?
C19 C11 C21 74.9(17) 5_556 5_556 ?
C19 C11 C12 51.3(13) 5_556 5_556 ?
C21 C11 C12 123.8(17) 5_556 5_556 ?
C19 C11 C12 156(2) 5_556 . ?
C21 C11 C12 124.6(17) 5_556 . ?
C12 C11 C12 111.6(13) 5_556 . ?
C19 C11 C11 105(2) 5_556 5_556 ?
C21 C11 C11 180(2) 5_556 5_556 ?
C12 C11 C11 56.5(12) 5_556 5_556 ?
C12 C11 C11 55.1(11) . 5_556 ?
C19 C12 C11 59.9(13) . 5_556 ?
C19 C12 C13 121.3(15) . . ?
C11 C12 C13 162.3(13) 5_556 . ?
C19 C12 C22 51.8(14) . . ?
C11 C12 C22 108.2(14) 5_556 . ?
C13 C12 C22 69.6(14) . . ?
C19 C12 C11 124.9(15) . . ?
C11 C12 C11 68.4(13) 5_556 . ?
C13 C12 C11 113.7(14) . . ?
C22 C12 C11 176.6(16) . . ?
C14 C13 C12 115(2) . . ?
C14 C13 C22 59.3(15) . . ?
C12 C13 C22 55.3(12) . . ?
C15 C14 C13 122(2) . . ?
C15 C14 C22 49.8(15) . . ?
C13 C14 C22 71.8(17) . . ?
C22 C15 C14 77.0(18) . . ?
C22 C15 C18 51.1(14) . . ?
C14 C15 C18 126.9(15) . . ?
C22 C15 C16 162(2) . . ?
C14 C15 C16 119.9(19) . . ?
C18 C15 C16 111.2(18) . . ?
C22 C15 C17 107.2(19) . . ?
C14 C15 C17 162.4(18) . . ?
C18 C15 C17 56.4(11) . . ?
C16 C15 C17 55.1(16) . . ?
C17 C16 C15 69.7(15) . . ?
C17 C16 C23 154.4(16) . . ?
C15 C16 C23 84.7(16) . . ?
C16 C17 C18 107.8(19) . . ?
C16 C17 C15 55.2(13) . . ?
C18 C17 C15 52.9(10) . . ?
C22 C18 C15 53.9(15) . . ?
C22 C18 C20 122.0(17) . . ?
C15 C18 C20 165.6(14) . . ?
C22 C18 C19 53.3(16) . . ?
C15 C18 C19 106.6(15) . . ?
C20 C18 C19 73.1(13) . . ?
C22 C18 C17 124.4(19) . . ?
C15 C18 C17 70.8(13) . . ?
C20 C18 C17 109.9(16) . . ?
C19 C18 C17 176.7(19) . . ?
C22 C19 C12 75(2) . . ?
C22 C19 C11 137(3) . 5_556 ?
C12 C19 C11 68.8(15) . 5_556 ?
C22 C19 C18 50.3(16) . . ?
C12 C19 C18 124.2(19) . . ?
C11 C19 C18 146(2) 5_556 . ?
C22 C19 C21 141(2) . . ?
C12 C19 C21 120.4(16) . . ?
C11 C19 C21 53.8(13) 5_556 . ?
C18 C19 C21 99.0(17) . . ?
C22 C19 C20 100(2) . . ?
C12 C19 C20 148(2) . . ?
C11 C19 C20 98.6(17) 5_556 . ?
C18 C19 C20 52.8(12) . . ?
C21 C19 C20 46.5(12) . . ?
C21 C20 C18 118.8(18) . . ?
C21 C20 C19 65.0(14) . . ?
C18 C20 C19 54.1(11) . . ?
C20 C21 C11 118(2) . 5_556 ?
C20 C21 O5 108.3(17) . . ?
C11 C21 O5 125.5(17) 5_556 . ?
C20 C21 C19 68.6(15) . . ?
C11 C21 C19 51.3(13) 5_556 . ?
O5 C21 C19 136.9(17) . . ?
C18 C22 C15 75.0(19) . . ?
C18 C22 C19 76(2) . . ?
C15 C22 C19 150(3) . . ?
C18 C22 C12 128(2) . . ?
C15 C22 C12 157(2) . . ?
C19 C22 C12 53.0(15) . . ?
C18 C22 C14 127(2) . . ?
C15 C22 C14 53.1(15) . . ?
C19 C22 C14 157(3) . . ?
C12 C22 C14 103.9(18) . . ?
C18 C22 C13 169(2) . . ?
C15 C22 C13 102.0(19) . . ?
C19 C22 C13 108(2) . . ?
C12 C22 C13 55.0(12) . . ?
C14 C22 C13 48.9(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt N1 1.999(9) . ?
Pt O2 2.000(8) . ?
Pt O1 2.012(7) . ?
Pt Cl 2.309(3) . ?
O1 C1 1.271(13) . ?
N1 C3 1.481(12) . ?
N1 C2 1.494(14) . ?
N1 C5 1.524(11) . ?
C1 O3 1.231(13) . ?
C1 C2 1.526(15) . ?
O2 C4 1.285(15) . ?
C3 C4 1.512(17) . ?
O4 C4 1.214(14) . ?
C5 C6 1.521(14) . ?
O5 C21 1.67(3) . ?
C6 C7 1.526(13) . ?
C7 C7 1.50(2) 7_556 ?
O7 O7 1.00(3) 2_556 ?
C11 C19 1.39(3) 5_556 ?
C11 C21 1.44(3) 5_556 ?
C11 C12 1.50(2) 5_556 ?
C11 C12 1.52(2) . ?
C11 C11 1.70(4) 5_556 ?
C12 C19 1.25(3) . ?
C12 C11 1.50(2) 5_556 ?
C12 C13 1.51(3) . ?
C12 C22 1.52(3) . ?
C13 C14 1.37(3) . ?
C13 C22 1.73(4) . ?
C14 C15 1.29(3) . ?
C14 C22 1.57(3) . ?
C15 C22 1.23(3) . ?
C15 C18 1.47(2) . ?
C15 C16 1.52(2) . ?
C15 C17 1.74(3) . ?
C16 C17 1.52(4) . ?
C16 C23 1.91(4) . ?
C17 C18 1.53(2) . ?
C18 C22 1.18(3) . ?
C18 C20 1.47(3) . ?
C18 C19 1.49(2) . ?
C19 C22 1.23(3) . ?
C19 C11 1.39(3) 5_556 ?
C19 C21 1.72(3) . ?
C19 C20 1.76(3) . ?
C20 C21 1.37(3) . ?
C21 C11 1.44(3) 5_556 ?
