A mixed-valence iron complex of the antitumour drug 6-mercaptopurine: tris(6-mercaptopurine)iron(II) tetrachloroferrate(III) chloride
Schmalle, Helmut W.; Gyr, Ernst; Dubler, Erich; Acta Crystallographica Section C 56 (2000) 957–959; doi:10.1107/S0108270100008118

data_2011286
_publ_section_title
;
 A mixed-valence iron complex of the antitumour drug 6-mercaptopurine:
 tris(6-mercaptopurine)iron(II) tetrachloroferrate(III) chloride
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              957
_journal_page_last               959
_journal_paper_doi               10.1107/S0108270100008118
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Fe (C5 H4 N4 S)3] [Fe Cl4] Cl'
_chemical_formula_moiety         'C15 H12 N12 S3 Fe, Fe Cl4, Cl'
_chemical_formula_sum            'C15 H12 Cl5 Fe2 N12 S3'
_chemical_formula_weight         745.50
_chemical_name_systematic
;
tris(1,6-dihydro-9H-purine-6-thione-N^7^,S)iron(II) tetrachloroferrate(III)
chloride
;
_space_group_IT_number           173
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.3499(6)
_cell_length_b                   10.3499(6)
_cell_length_c                   14.6652(11)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      3.6
_cell_volume                     1360.48(15)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED in IPDS'
_computing_molecular_graphics    'PLATON (Spek, 1990) and PLUTON (Spek, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full .993
_diffrn_measured_fraction_theta_max .993
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '\f rotation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .031
_diffrn_reflns_av_sigmaI/netI    .035
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16156
_diffrn_reflns_theta_full        30.35
_diffrn_reflns_theta_max         30.35
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  3.5
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  .669
_exptl_absorpt_correction_T_min  .630
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             742
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .24
_refine_diff_density_max         .26
_refine_diff_density_min         -.24
_refine_ls_abs_structure_details 'Flack (1983); 1306 Friedel pairs'
_refine_ls_abs_structure_Flack   -.05(2)
_refine_ls_extinction_coef       .0107(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2717
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          .024
_refine_ls_R_factor_gt           .021
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.01P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .038
_reflns_number_gt                2484
_reflns_number_total             2717
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1395.cif
_cod_data_source_block           I
_cod_database_code               2011286
_cod_database_fobs_code          2011286