Heterotrinuclear Complexes with Palladium, Rhodium, and Iridium Ions Assembled by Conformational Switching of a Tetraphosphine Ligand around a Palladium Center
Yoshii, Akiko; Takenaka, Hiroe; Nagata, Hiroko; Noda, Sayo; Nakamae, Kanako; Kure, Bunsho; Nakajima, Takayuki; Tanase, Tomoaki; Organometallics 31 (2012) 133–; doi:10.1021/om2006744

data_4067809
_publ_section_title
;
 Heterotrinuclear Complexes with Palladium, Rhodium, and Iridium Ions
 Assembled by Conformational Switching of a Tetraphosphine Ligand around a
 Palladium Center
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              133
_journal_paper_doi               10.1021/om2006744
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C61 H70 Cl10 Ir P4 Pd Rh '
_chemical_formula_sum            'C61 H70 Cl10 Ir P4 Pd Rh'
_chemical_formula_weight         1683.17
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   23.3351(7)
_cell_length_b                   15.3353(4)
_cell_length_c                   18.1485(6)
_cell_measurement_reflns_used    15317
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     6494.5(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Mercury 2.4'
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55897
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    3.122
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3336.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.96
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6438 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     713
_refine_ls_number_reflns         13818
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                13247
_reflns_number_total             13818
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om2006744_si_002.cif
_cod_data_source_block           '_complex31c'
_cod_original_formula_sum        'C61 H70 Cl10 Ir P4 Pd Rh '
_cod_database_code               4067809