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_4116816
_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 H48 N10 O8 Pt4, (N O3)6, (H2 O)4'
_chemical_formula_sum            'C16 H56 N16 O30 Pt4'
_chemical_formula_weight         1733.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                106.41(2)
_cell_angle_beta                 92.20(2)
_cell_angle_gamma                100.92(2)
_cell_formula_units_Z            1.00
_cell_length_a                   10.492(3)
_cell_length_b                   11.864(3)
_cell_length_c                   9.856(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      20.13
_cell_volume                     1150.0(5)
_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      -0.01196
_diffrn_orient_matrix_UB_12      -0.08934
_diffrn_orient_matrix_UB_13      -0.03715
_diffrn_orient_matrix_UB_21      0.03465
_diffrn_orient_matrix_UB_22      -0.00230
_diffrn_orient_matrix_UB_23      0.09490
_diffrn_orient_matrix_UB_31      -0.09038
_diffrn_orient_matrix_UB_32      -0.00931
_diffrn_orient_matrix_UB_33      0.03012
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7043
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        -0.74
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.235
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5384
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'psi-scan (North's method)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.5023
_exptl_crystal_description       plate
_exptl_crystal_F_000             816.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.47
_refine_diff_density_min         -2.19
_refine_ls_abs_structure_details
;
none
;
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     noref
_refine_ls_goodness_of_fit_obs   1.270
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    5
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_obs          0.0445
_refine_ls_shift/esd_max         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma_w=1/\s^2^(F)
_refine_ls_wR_factor_all         0.0350
_refine_ls_wR_factor_obs         0.0314
_reflns_number_observed          5002
_reflns_number_total             6704
_reflns_observed_criterion       I_>_2.0_sigma(I)
_cod_data_source_file            ja980019q_8.cif
_cod_data_source_block           complex14
_cod_original_cell_volume        1150.1(5)
_cod_database_code               4116816