#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304663.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_4304663
loop_
_publ_author_name
'Rosa Ranaldo'
'Nicola Margiotta'
'Francesco P. Intini'
'Concetta Pacifico'
'Giovanni Natile'
_publ_contact_author_address
;
Dipartimento farmaco-Chimico
Università di Bari
via E. Orabona 4
70125 Bari 
Italy

;
_publ_contact_author_email       natile@farmchim.uniba.it
_publ_contact_author_fax         '39 80 5442230'
_publ_contact_author_name
;
Prof Giovanni Natile
;
_publ_contact_author_phone       '39 80 5442774'
_publ_section_title
;
Conformer Distribution in
(cis-1,4-DACH)bis(guanosine-5'-phosphate)platinum(II) Adducts: A Reliable
Model for DNA Adducts of Antitumoral Cisplatin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2820
_journal_page_last               2830
_journal_paper_doi               10.1021/ic702202x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C9 H21 Cl2 N3 O Pt'
_chemical_formula_weight         453.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 111.747(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9138(4)
_cell_length_b                   13.2679(4)
_cell_length_c                   9.3672(3)
_cell_measurement_reflns_used    27693
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.40
_cell_volume                     1375.30(8)
_computing_cell_refinement       'SAINT-IRIX  (Bruker, 2004)'
_computing_data_collection       'COSMO, APEX2 and BIS (Bruker, 2004)'
_computing_data_reduction        'SAINT-IRIX  (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (L. J Farrugia, 1997)'
_computing_publication_material
;
PARST97 (M. Nardelli,  1983; M. Nardelli, 1995.), WinGX  (L. J. Farrugia, 
1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (M. C. Burla et al. 2003)''
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'BrukerAXS X8 APEX CCD system'
_diffrn_measurement_method       'φ and ω'
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27693
_diffrn_reflns_theta_full        33.10
_diffrn_reflns_theta_max         33.10
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.576
_exptl_absorpt_correction_T_max  0.4224
_exptl_absorpt_correction_T_min  0.0190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; G.M. Sheldrick, 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.335
_refine_diff_density_min         -2.545
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0353P)²+1.3642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                3651
_reflns_number_total             5150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702202x-file001.cif
_cod_data_source_block           rosita1
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304663
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pt1 Pt 0.412027(18) 0.107884(13) 0.49232(2) 0.02633(7) Uani 1 1 d . . .
Cl1 Cl 0.58258(14) 0.20723(11) 0.53719(18) 0.0414(3) Uani 1 1 d . . .
Cl2 Cl 0.37260(16) 0.09481(11) 0.23066(16) 0.0429(4) Uani 1 1 d . . .
N1 N 0.2639(4) 0.0160(3) 0.4471(5) 0.0311(10) Uani 1 1 d . B .
H1A H 0.2095 0.0367 0.3562 0.037 Uiso 1 1 calc R . .
H1B H 0.2877 -0.0459 0.4309 0.037 Uiso 1 1 calc R . .
N2 N 0.4496(5) 0.1241(4) 0.7235(5) 0.0391(12) Uani 1 1 d . . .
H2A H 0.5129 0.0835 0.7714 0.047 Uiso 1 1 calc R . .
H2B H 0.4765 0.1876 0.7473 0.047 Uiso 1 1 calc R . .
C1 C 0.1956(7) 0.0018(7) 0.5494(8) 0.064(2) Uani 1 1 d . . .
H1 H 0.1164 -0.0237 0.4826 0.076 Uiso 1 1 calc R A 1
C2A C 0.1700(18) 0.1282(14) 0.588(2) 0.042(4) Uani 0.44 1 d P B 1
H2A1 H 0.1894 0.1735 0.5194 0.051 Uiso 0.44 1 calc PR B 1
H2A2 H 0.0860 0.1380 0.5750 0.051 Uiso 0.44 1 calc PR B 1
C3A C 0.2531(18) 0.1485(14) 0.756(2) 0.039(4) Uani 0.44 1 d P B 1
H3A1 H 0.2633 0.2207 0.7707 0.047 Uiso 0.44 1 calc PR B 1
H3A2 H 0.2129 0.1245 0.8227 0.047 Uiso 0.44 1 calc PR B 1
C6A C 0.2252(18) -0.0513(11) 0.6689(19) 0.040(4) Uani 0.44 1 d P B 1
H6A1 H 0.2251 -0.1216 0.6402 0.049 Uiso 0.44 1 calc PR B 1
H6A2 H 0.1646 -0.0433 0.7144 0.049 Uiso 0.44 1 calc PR B 1
C5A C 0.3441(18) -0.0266(12) 0.785(2) 0.046(4) Uani 0.44 1 d P B 1
H5A1 H 0.4072 -0.0555 0.7558 0.055 Uiso 0.44 1 calc PR B 1
H5A2 H 0.3512 -0.0548 0.8835 0.055 Uiso 0.44 1 calc PR B 1
C2 C 0.1454(12) 0.0771(11) 0.5919(16) 0.043(3) Uani 0.56 1 d P B 2
H21 H 0.1062 0.0517 0.6588 0.052 Uiso 0.56 1 calc PR B 2
H22 H 0.0830 0.1050 0.5015 0.052 Uiso 0.56 1 calc PR B 2
C3 C 0.2315(17) 0.1621(11) 0.676(2) 0.050(4) Uani 0.56 1 d P B 2
H31 H 0.1949 0.2037 0.7317 0.060 Uiso 0.56 1 calc PR B 2
H32 H 0.2498 0.2042 0.6025 0.060 Uiso 0.56 1 calc PR B 2
C5 C 0.3418(13) 0.0132(10) 0.8378(13) 0.039(3) Uani 0.56 1 d P B 2
H51 H 0.2828 0.0159 0.8866 0.047 Uiso 0.56 1 calc PR B 2
H52 H 0.4166 -0.0123 0.9132 0.047 Uiso 0.56 1 calc PR B 2
C6 C 0.2969(14) -0.0621(10) 0.7035(15) 0.036(3) Uani 0.56 1 d P B 2
H61 H 0.2578 -0.1192 0.7306 0.044 Uiso 0.56 1 calc PR B 2
H62 H 0.3641 -0.0868 0.6786 0.044 Uiso 0.56 1 calc PR B 2
C4 C 0.3609(8) 0.1065(6) 0.8002(8) 0.060(2) Uani 1 1 d . . .
H4 H 0.4025 0.1222 0.9094 0.072 Uiso 1 1 calc R B 1
C7 C 0.0387(7) 0.3843(5) 0.5728(9) 0.0486(16) Uani 1 1 d . . .
H7 H 0.126(7) 0.371(5) 0.556(7) 0.045(17) Uiso 1 1 d . . .
C8 C -0.1760(7) 0.3571(7) 0.4626(8) 0.0575(19) Uani 1 1 d . . .
H8A H -0.2191 0.4092 0.3925 0.086 Uiso 1 1 calc R . .
H8B H -0.1704 0.3743 0.5646 0.086 Uiso 1 1 calc R . .
H8C H -0.2183 0.2944 0.4326 0.086 Uiso 1 1 calc R . .
C9 C -0.0473(8) 0.3063(6) 0.3210(8) 0.063(2) Uani 1 1 d . . .
H9A H 0.0362 0.3023 0.3331 0.095 Uiso 1 1 calc R . .
H9B H -0.0898 0.3492 0.2355 0.095 Uiso 1 1 calc R . .
H9C H -0.0823 0.2401 0.3027 0.095 Uiso 1 1 calc R . .
O1 O 0.0360(5) 0.4237(4) 0.6905(6) 0.0636(14) Uani 1 1 d . . .
N3 N -0.0564(5) 0.3475(4) 0.4600(5) 0.0383(11) Uani 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N2 Pt1 N1 96.57(18) . . ?
N2 Pt1 Cl2 178.06(15) . . ?
N1 Pt1 Cl2 85.16(12) . . ?
N2 Pt1 Cl1 85.16(14) . . ?
N1 Pt1 Cl1 177.53(13) . . ?
Cl2 Pt1 Cl1 93.13(6) . . ?
C1 N1 Pt1 125.2(4) . . ?
C4 N2 Pt1 124.9(4) . . ?
C6A C1 C2 99.6(10) . . ?
C6A C1 N1 127.4(11) . . ?
C2 C1 N1 121.8(9) . . ?
C6A C1 C6 25.9(8) . . ?
C2 C1 C6 112.4(8) . . ?
N1 C1 C6 102.9(7) . . ?
C6A C1 C2A 111.2(10) . . ?
C2 C1 C2A 22.1(8) . . ?
N1 C1 C2A 101.0(7) . . ?
C6 C1 C2A 114.6(9) . . ?
C3A C2A C1 106.3(12) . . ?
C4 C3A C2A 115.4(14) . . ?
C1 C6A C5A 114.2(14) . . ?
C6A C5A C4 109.3(11) . . ?
C1 C2 C3 115.2(12) . . ?
C2 C3 C4 107.1(10) . . ?
C4 C5 C6 115.4(10) . . ?
C5 C6 C1 106.8(10) . . ?
C3A C4 C5 103.5(11) . . ?
C3A C4 N2 124.2(10) . . ?
C5 C4 N2 119.5(9) . . ?
C3A C4 C3 23.1(8) . . ?
C5 C4 C3 112.4(9) . . ?
N2 C4 C3 102.8(7) . . ?
C3A C4 C5A 109.0(11) . . ?
C5 C4 C5A 21.7(7) . . ?
N2 C4 C5A 101.3(8) . . ?
C3 C4 C5A 109.0(9) . . ?
O1 C7 N3 125.0(7) . . ?
C7 N3 C8 120.9(6) . . ?
C7 N3 C9 121.9(6) . . ?
C8 N3 C9 116.9(6) . . ?
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
Pt1 N2 2.054(5) . ?
Pt1 N1 2.056(4) . ?
Pt1 Cl2 2.3248(14) . ?
Pt1 Cl1 2.3259(14) . ?
N1 C1 1.481(7) . ?
N2 C4 1.499(8) . ?
C1 C6A 1.258(17) . ?
C1 C2 1.300(15) . ?
C1 C6 1.723(16) . ?
C1 C2A 1.77(2) . ?
C2A C3A 1.54(2) . ?
C3A C4 1.32(2) . ?
C6A C5A 1.47(3) . ?
C5A C4 1.777(18) . ?
C2 C3 1.53(2) . ?
C3 C4 1.72(2) . ?
C5 C4 1.330(13) . ?
C5 C6 1.539(16) . ?
C7 O1 1.231(9) . ?
C7 N3 1.324(9) . ?
C8 N3 1.440(9) . ?
C9 N3 1.452(8) . ?
