New Structural Aspects of α-Pyrrolidinonate- and α-Pyridonate-Bridged, Homo- and Mixed-Valence, Di- and Tetranuclear cis-Diammineplatinum Complexes: Eight New Crystal Structures, Stoichiometric 1:1 Mixture of Pt(2.25+)4 and Pt(2.5+)4, New Quasi-One-Dimensional Halide-Bridged [Pt(2.5+)4-Cl...]∞System, and Consideration of Solution Properties
Ken Sakai; Yuko Tanaka; Yuriko Tsuchiya; Kentaro Hirata; Taro Tsubomura; Seiichiro Iijima; Ashis Bhattacharjee; Journal of the American Chemical Society 120 (1998) 8366–8379; doi:10.1021/ja980019q

data_4116813
_publ_contact_author
;
    Dr Ken Sakai
    Department of Industrial Chemistry
    Faculty of Engineering
    Seikei University
    Kichijoji-Kitamachi
    Musashino, Tokyo 180
    Japan
;
_publ_contact_author_email       ksakai@ch.seikei.ac.jp
_publ_contact_author_fax         '+81 422 37 3871'
_publ_contact_author_phone       '+81 422 37 3759'
_publ_section_title
;
 New Structural Aspects of \a-Pyrrolidinonate- and \a-Pyridonate-Bridged,
 Homo- and Mixed-Valence, Di- and Tetranuclear cis-Diammineplatinum
 Complexes: Eight New Crystal Structures, Stoichiometric 1:1 Mixture of
 Pt(2.25+)4 and Pt(2.5+)4, New Quasi-One-Dimensional Halide-Bridged
 [Pt(2.5+)4-Cl...]\\infty System, and Consideration of Solution Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8366
_journal_page_last               8379
_journal_paper_doi               10.1021/ja980019q
_journal_volume                  120
_journal_year                    1998
_chemical_formula_moiety         'C16 Cl H48 N12 O4 Pt4, Cl2, (Cl O4)3'
_chemical_formula_sum            'C16 H48 Cl6 N12 O16 Pt4'
_chemical_formula_weight         1657.704
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             1997-10-28
_audit_creation_method           'teXsan (modified by Ken Sakai)'
_audit_update_record
;
1997-10-28    text and data added by Ken Sakai
;
_cell_angle_alpha                90
_cell_angle_beta                 95.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   9.999(5)
_cell_length_b                   26.98(1)
_cell_length_c                   17.427(4)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      17.65
_cell_measurement_theta_min      7.21
_cell_volume                     4682(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SIR88
_diffrn_ambient_temperature      296.0
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \q/2\q
_diffrn_orient_matrix_UB_11      -0.08344
_diffrn_orient_matrix_UB_12      0.00894
_diffrn_orient_matrix_UB_13      0.02438
_diffrn_orient_matrix_UB_21      -0.02184
_diffrn_orient_matrix_UB_22      -0.03596
_diffrn_orient_matrix_UB_23      0.00506
_diffrn_orient_matrix_UB_31      0.05144
_diffrn_orient_matrix_UB_32      -0.00073
_diffrn_orient_matrix_UB_33      0.05196
_diffrn_radiation_detector       'scintillation,NaI,Rigaku SC-30'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.3333
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7358
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        -6.21
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.323
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9031
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.3518
_exptl_crystal_description       'thin plate-needle'
_exptl_crystal_F_000             3080.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.53
_refine_diff_density_min         -2.66
_refine_ls_abs_structure_details
;
none
;
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     noref
_refine_ls_goodness_of_fit_obs   1.530
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3045
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2704
_refine_ls_R_factor_obs          0.1019
_refine_ls_shift/esd_max         0.5980
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma_w=1/\s^2^(F)+0.000400F^2^
_refine_ls_wR_factor_all         0.1269
_refine_ls_wR_factor_obs         0.0950
_reflns_number_observed          3045
_reflns_number_total             7339
_reflns_observed_criterion       I_>_2.0_sigma(I)
_cod_data_source_file            ja980019q_5.cif
_cod_data_source_block           complex9
_cod_original_formula_sum        'C16 Cl6 H48 N12 O16 Pt4'
_cod_database_code               4116813