Complexes of Platinum(II) Containing Neutral and Deprotonated 9-Methyladenine. Synthesis, X-ray Structures, and NMR Studies on the Cyclic Trimer cis-[L2Pt{9-MeAd(-H)}]3(NO3)3 and the Dinuclear cis-[L2Pt(ONO2){9-MeAd(-H)}PtL2](NO3)2 (L = PMePh2)
Bruno Longato; Lucia Pasquato; Adele Mucci; Luisa Schenetti; Ennio Zangrando; Inorganic Chemistry 42 (2003) 7861–7871; doi:10.1021/ic034406z

data_4312578
_publ_section_title
;
 Complexes of Platinum(II) Containing Neutral and Deprotonated
 9-Methyladenine. Synthesis, X-ray Structures, and NMR Studies on the
 Cyclic Trimer cis-[L2Pt{9-MeAd(-H)}]3(NO3)3 and the Dinuclear
 cis-[L2Pt(ONO2){9-MeAd(-H)}PtL2](NO3)2 (L = PMePh2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7861
_journal_page_last               7871
_journal_paper_doi               10.1021/ic034406z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'(C96 H96 N15 P6 Pt3 3+) 3(N1 O3 1-) 0.75(H2 O)'
_chemical_formula_sum            'C96 H97.5 N18 O9.75 P6 Pt3'
_chemical_formula_weight         2430.51
_chemical_name_systematic
;
   exa(methyl-diphenyl-phosphine)-tris(9-methyl-adenine(-H))-
   tri-platinum(II) tris(nitrate) hydrated
;
_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                 93.58(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.144(6)
_cell_length_b                   18.216(4)
_cell_length_c                   36.300(6)
_cell_measurement_temperature    100(2)
_cell_volume                     19894(7)
_computing_cell_refinement       'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_reduction        'Scala (Acta Cryst. D50, 760, 1994)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.64.04 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'CCD MarResearch'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0000
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            47103
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    7.003
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_correction_T_min  0.5019
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9612
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         25020
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+161.46P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2184
_reflns_number_gt                20185
_reflns_number_total             25026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034406z.cif
_cod_data_source_block           2
_cod_original_cell_volume        19893(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C96 H97.50 N18 O9.75 P6 Pt3'
_cod_database_code               4312578