NMR and X-ray Structural Characterization of a Cisplatin Analogue Able To Slow Down the Pt-N7 Rotation of a Coordinated Guanine Base by a Billion-Fold Times: 2,2'-Bipiperidine(dimethylmalonato)platinum(II) Complex
Francesco P. Intini; Renzo Cini; Gabriella Tamasi; Michael B. Hursthouse; Giovanni Natile; Inorganic Chemistry 47 (2008) 4909–4917; doi:10.1021/ic800230p

data_4305042
_publ_contact_author_address     'Dipartimento Farmaco-Chimico Univ di Bari'
_publ_contact_author_email       natile@farmchim.uniba.it
_publ_contact_author_fax         '+39 080 5442 230'
_publ_contact_author_name        'Prof Giovanni Natile'
_publ_contact_author_phone       '+39 080 5442 774'
_publ_section_title
;
NMR and X-ray Structural Characterization of a Cisplatin Analogue Able To
Slow Down the Pt-N7 Rotation of a Coordinated Guanine Base by a
Billion-Fold Times: 2,2'-Bipiperidine(dimethylmalonato)platinum(II)
Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4909
_journal_page_last               4917
_journal_paper_doi               10.1021/ic800230p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C15 H26 N2 O4 Pt, 4 (H2 O)'
_chemical_formula_sum            'C15 H34 N2 O8 Pt'
_chemical_formula_weight         565.52
_chemical_name_common            '[Pt(II)(dmm)(bip)] 4H2O'
_chemical_name_systematic
;
 [Pt(II)(Dimethylmalonato)((+/-)2,2'-Bipiperidine)] Tetra-hydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 106.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.078(3)
_cell_length_b                   15.063(3)
_cell_length_c                   10.485(2)
_cell_measurement_reflns_used    2182
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     1976.3(8)
_computing_cell_refinement
;
 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
;
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
;
 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
;
_computing_molecular_graphics    'ORTEP-32 (Farrugia, 1998)'
_computing_publication_material  'CIFTAB  (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
'Bruker-Nonius 95mm CCD camera on \k-goniostat' 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8916
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.143
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00112(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.759
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.760
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+10.7076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                2288
_reflns_number_total             2350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800230p-file003.cif
_cod_data_source_block           pt1lab
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1976.3(7)
_cod_original_formula_sum        'C15 H34 N2 O8 Pt1'
_cod_database_code               4305042