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_4067805
_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         'C54 H63 Cl5 F6 O P5 Pd Rh '
_chemical_formula_sum            'C54 H63 Cl5 F6 O P5 Pd Rh'
_chemical_formula_weight         1383.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.395(4)
_cell_angle_beta                 108.107(4)
_cell_angle_gamma                109.1568(15)
_cell_formula_units_Z            2
_cell_length_a                   12.242(4)
_cell_length_b                   15.428(5)
_cell_length_c                   17.398(6)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2928.5(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP-II
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27350
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangularplate
_exptl_crystal_F_000             1400.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.54
_refine_diff_density_min         -1.01
_refine_ls_extinction_coef       0.0023(7)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     671
_refine_ls_number_reflns         12938
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1279P)^2^+1.5587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2489
_reflns_number_gt                7736
_reflns_number_total             12938
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om2006744_si_002.cif
_cod_data_source_block           '_complex23a'
_cod_original_cell_volume        2928.3(16)
_cod_original_formula_sum        'C54 H63 Cl5 F6 O P5 Pd Rh '
_cod_database_code               4067805