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_4313748
_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_moiety         'C18 H18 N12 Pd3 '
_chemical_formula_sum            'C18 H18 N12 Pd3'
_chemical_formula_weight         721.62
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.9731(2)
_cell_length_b                   16.9731(2)
_cell_length_c                   30.6315(7)
_cell_measurement_reflns_used    16818
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     8824.5(2)
_computing_cell_refinement       D*TREK
_computing_data_collection       D*TREK
_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_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device_type  'Quantum CCD/Rigaku AFC7'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            40193
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            ' pale yellow '
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.2Ueq(C)'
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5057
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.01000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                3747
_reflns_number_total             5057
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic026196g_2.cif
_cod_data_source_block           Pd3(pz)6
_cod_original_cell_volume        8824.5(3)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C18 H18 N12 Pd3 '
_cod_database_code               4313748