Mono- and di-nuclear complexes of (trpy)MII (M = Pd, Pt) with the model nucleobase 1-methylcytosine. Crystal structure and NMR solution studies
Coşar, Sultan; Janik, Matthias B. L.; Flock, Matthias; Freisinger, Eva; Farkas, Etelka; Lippert, Bernhard; Journal of the Chemical Society, Dalton Transactions  (1999) 2329–; doi:10.1039/a902862e

data_7027448
_publ_section_title
;
 Mono- and di-nuclear complexes of (trpy)MII (M = Pd, Pt) with the model 
 nucleobase 1-methylcytosine. Crystal structure and NMR solution studies
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2329
_journal_paper_doi               10.1039/a902862e
_journal_year                    1999
_chemical_formula_sum            'C35 H30 Cl3 N9 O14 Pd2'
_chemical_formula_weight         1119.83
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.309(3)
_cell_length_b                   10.961(2)
_cell_length_c                   25.975(5)
_cell_measurement_reflns_used    11271
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      4.66
_cell_volume                     3999.8(14)
_computing_cell_refinement       'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius BV, Netherlands)'
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via \w-rotation (\D\w\=1\%) and two times 22s per frame
;
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11271
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.7567
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       cube
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00004(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.864
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    'refU, except H4 refall'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_obs          0.0439
_refine_ls_shift/esd_max         1.331
_refine_ls_shift/esd_mean        0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1137
_refine_ls_wR_factor_obs         0.0954
_reflns_number_observed          2980
_reflns_number_total             5838
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902862Esup1.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] 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^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027448