Synthesis and Characterization of Cyclotetraphosphato Complexes of Rh(I), Ir(I), Ru(II), and Pd(II)
Sou Kamimura; Shigeki Kuwata; Masakazu Iwasaki; Youichi Ishii; Inorganic Chemistry 43 (2004) 399–401; doi:10.1021/ic0350382

data_4310463
_publ_contact_author_address
;
     Department of Applied Chemistry, Faculty of Science and Engineering,
     Chuo University, Kasuga, Bunkyo-ku, Tokyo 112-8551, Japan
;
_publ_contact_author_email       ' ishii@chem.chuo-u.ac.jp '
_publ_contact_author_fax         ' +81-3-3817-1895 '
_publ_contact_author_name        ' Youichi Ishii'
_publ_contact_author_phone       ' +81-3-3817-1901 '
_publ_section_title
;
 Synthesis and Characterization of Cyclotetraphosphato Complexes of Rh(I),
 Ir(I), Ru(II), and Pd(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              399
_journal_page_last               401
_journal_paper_doi               10.1021/ic0350382
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C80 H78 N2 O14 P8 Pd2'
_chemical_formula_weight         1752.09
_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             'Mon Apr  7 22:36:57 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 99.17(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.128(6)
_cell_length_b                   16.224(7)
_cell_length_c                   24.311(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      19.6
_cell_measurement_theta_min      18.5
_cell_volume                     3944(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9564
_diffrn_standards_decay_%        4.09
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            paleyellowXDIM
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       XDIM
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     487
_refine_ls_number_reflns         4390
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.0100
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00011|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                4390
_reflns_number_total             9062
_cod_data_source_file            ic0350382si20031208_102540_6.cif
_cod_data_source_block           (PPN)2[{Pd(C3H5)}2(P4O12)](6)
_cod_original_cell_volume        3943(3)
_cod_original_formula_sum        'C80 H78 N2 O14 P8 Pd2 '
_cod_database_code               4310463
_reflns_threshold_criterion      F^2^>3.0\s(F^2^)