Dynamic processes in platinum(II)‒adenosine complexes. Preparation, NMR spectroscopic characterisation and crystal structure of isomeric PtII(dien)‒adenosine complexes
Arpalahti, Jorma; Klika, Karel D.; Sillanpää, Reijo; Kivekäs, Raikko; Journal of the Chemical Society, Dalton Transactions  (1998) 1397–; doi:10.1039/a708955d

data_7027986
_publ_section_title
;
 Dynamic processes in platinum(II)--adenosine complexes. Preparation, NMR
 spectroscopic characterisation and crystal structure of isomeric
 PtII(dien)--adenosine complexes
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1397
_journal_paper_doi               10.1039/a708955d
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety
;  
2(C14 H31 N8 O4 Pt), 4(Cl O4), 5.54(H2 O)  
;
_chemical_formula_structural     'C14 H31.54 Cl2 N8 O14.77 Pt'
_chemical_formula_sum            'C14 H31.54 Cl2 N8 O14.77 Pt'
_chemical_formula_weight         814.32
_chemical_melting_point          ?
_chemical_name_systematic
;   
 ?   
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.170(10)
_cell_angle_beta                 108.40(2)
_cell_angle_gamma                70.95(2)
_cell_formula_units_Z            2
_cell_length_a                   12.167(4)
_cell_length_b                   14.644(2)
_cell_length_c                   8.746(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      20.06
_cell_measurement_theta_min      18.03
_cell_volume                     1375.6(6)
_computing_cell_refinement
;  
Molecular Structure Corporation (1995), MSC/AFC Diffractomer
Controll Software. MSC, 3200 Research Forest Drive, The 
Woodlands, TX 77381, USA. 
;
_computing_data_collection
;  
Molecular Structure Corporation (1995), MSC/AFC Diffractomer
Controll Software. MSC, 3200 Research Forest Drive, The 
Woodlands, TX 77381, USA. 
;
_computing_data_reduction
;  
Molecular Structure Corporation (1989), TEXSAN. Single Crystal
Structure Analysis Software. Version 5.0. MSC, 3200 Research 
Forest Drive, The Woodlands, TX 77381, USA.
;
_computing_molecular_graphics
;
ORTEPII (Johnson, C.K (1976). Report ORNL-5138. Oak Ridge National 
Laboratory, Tennessee, USA)
;
_computing_publication_material
;
SHELXL-92 (Sheldrick, G. M. (1993). Program for the Crystal 
Structure Refinement. University of G\"ottingen, Germany.
;
_computing_structure_refinement
;
SHELXL-92 (Sheldrick, G. M. (1993). Program for the Crystal 
Structure Refinement. University of G\"ottingen, Germany.
;
_computing_structure_solution
;
SHELXS-86 (Sheldrick, G. M. (1985). Program for the Solution of Crystal 
Structures. University of G\"ottingen, Germany.
;
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       w\--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6631
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type
;
empirical via \y scans (North, A.C.T., Phillips, D. C. & Mathews, F. S. 
(1968).Acta Cryst. A24, 351-359.)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             803
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6626
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_obs          0.0438
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+3.8370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1160
_refine_ls_wR_factor_obs         0.1057
_reflns_number_observed          5422
_reflns_number_total             6627
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d708955sup1.cif
_cod_data_source_block           '[Pt(dien)(Ado-N1)](ClO4)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+3.8370P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+3.8370P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7027986