Syntheses and Structures of Bridge and Chelate Isomers of Tetraplatinum(II) Cluster Complex with Diethyldithiophosphate Ion (Et2dtp) at In-Plane Sites, [Pt4(CH3COO)4(Et2dtp)4], and Their Mutual Isomerization via Cluster Core Rotation
Tadashi Yamaguchi; Haruko Saito; Taro Maki; Tasuku Ito; Journal of the American Chemical Society 121 (1999) 10738–10742; doi:10.1021/ja990596u

data_4116602
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
Tohoku University,Sendai  980-8578, JAPAN
;
_publ_contact_author_email       ' Ito@agnus.chem.tohoku.ac.jp '
_publ_contact_author_fax         ' +81 22 217 6548 '
_publ_contact_author_name        ' Tasuku ITO '
_publ_contact_author_phone       ' +81 22 217 6544 '
_publ_section_title
;
 Syntheses and Structures of Bridge and Chelate Isomers of
 Tetraplatinum(II) Cluster Complex with Diethyldithiophosphate Ion
 (Et2dtp) at In-Plane Sites, [Pt4(CH3COO)4(Et2dtp)4], and Their Mutual
 Isomerization via Cluster Core Rotation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10738
_journal_page_last               10742
_journal_paper_doi               10.1021/ja990596u
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C24 H52 O16 P4 Pt4 S8 '
_chemical_formula_sum            'C24 H52 O16 P4 Pt4 S8'
_chemical_formula_weight         1757.40
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             'Sun Dec 27 16:22:59 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.794(8)
_cell_length_b                   24.990(3)
_cell_length_c                   14.927(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.8
_cell_volume                     4772(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00580
_diffrn_orient_matrix_UB_12      -0.03929
_diffrn_orient_matrix_UB_13      0.01166
_diffrn_orient_matrix_UB_21      -0.00284
_diffrn_orient_matrix_UB_22      -0.00708
_diffrn_orient_matrix_UB_23      -0.06589
_diffrn_orient_matrix_UB_31      0.07789
_diffrn_orient_matrix_UB_32      0.00267
_diffrn_orient_matrix_UB_33      -0.00327
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.352
_diffrn_reflns_av_sigmaI/netI    0.083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5508
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        -2.18
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.183
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3296.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       0.00018(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.477
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0192
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0374
_reflns_number_gt                4052
_reflns_number_total             5507
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja990596u_2.cif
_cod_data_source_block           '[Pt4(OAc)4(dtp)4]_fr.2'
_cod_original_cell_volume        4772(2)
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C24 H52 O16 P4 Pt4 S8 '
_cod_database_code               4116602