Platinum-Modified Adenines: Unprecedented Protonation Behavior Revealed by NMR Spectroscopy and Relativistic Density-Functional Theory Calculations
Jan Vícha; Gabriel Demo; Radek Marek; Inorganic Chemistry 51 (2012) 1371–1379; doi:10.1021/ic201595e

data_4328123
_publ_contact_author_address
;
National Centre for Biomolecular Research and CEITEC
Masaryk University
Kamenice 5
Brno-Bohunice, 625 00, Czech Republic
;
_publ_contact_author_email       rmarek@chemi.muni.cz
_publ_contact_author_fax         '+420 549 492 556'
_publ_contact_author_name        'Radek Marek'
_publ_contact_author_phone       '+420 549 495 748'
_publ_section_title
;
 Platinum-Modified Adenines: Unprecedented Protonation Behavior Revealed
 by NMR Spectroscopy and Relativistic Density-Functional Theory
 Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1371
_journal_page_last               1379
_journal_paper_doi               10.1021/ic201595e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C12 H12 Cl5 N5 Pt, 2(C3 H7 N O)'
_chemical_formula_sum            'C18 H26 Cl5 N7 O2 Pt'
_chemical_formula_weight         744.80
_chemical_name_common
'9-[6-(benzylamino)purine] pentachloroplatinate (IV)'
_chemical_name_systematic
; 
9-[6-(benzylamino)purine] pentachloroplatinate (IV) 
;
_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'
_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                 100.496(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1279(4)
_cell_length_b                   8.3336(3)
_cell_length_c                   20.7956(6)
_cell_measurement_reflns_used    4528
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.05
_cell_volume                     2577.83(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>,  2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir 2002 (Burla <i>et al.</i>, 2000)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29609
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.992
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED (Oxford Diffraction Ltd, 2009).
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.649
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0228
_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/[\s^2^(Fo^2^)+(0.0368P)^2^+0.9795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                3875
_reflns_number_total             4528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201595e_si_002.cif
_cod_data_source_block           pt2
_cod_database_code               4328123