Pyrazolato-Bridged Polynuclear Palladium and Platinum Complexes. Synthesis, Structure, and Reactivity
Umakoshi, Keisuke; Yamauchi, Yoko; Nakamiya, Keiko; Kojima, Takashi; Yamasaki, Mikio; Kawano, Hiroyuki; Onishi, Masayoshi; Inorganic Chemistry 42 (2003) 3907–3916; doi:10.1021/ic026196g

data_4313750
_publ_section_title
;
 Pyrazolato-Bridged Polynuclear Palladium and Platinum Complexes.
 Synthesis, Structure, and Reactivity
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3907
_journal_page_last               3916
_journal_paper_doi               10.1021/ic026196g
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C28 H30 N14 Pd3'
_chemical_formula_weight         881.84
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.107(2)
_cell_length_b                   16.113(2)
_cell_length_c                   25.721(3)
_cell_measurement_reflns_used    23780
_cell_measurement_temperature    133.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     6675.4(14)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9728
_diffrn_measured_fraction_theta_max 0.9728
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            53982
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.2Ueq(C)'
_refine_ls_number_parameters     810
_refine_ls_number_reflns         12056
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                11324
_reflns_number_total             7612
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic026196g_4.cif
_cod_data_source_block           '_(Pd3(4Mepz)6).2CH3CN'
_cod_original_cell_volume        6675(1)
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C28 H30 N14 Pd3 '
_cod_database_code               4313750