A distorted square-planar Pd^<b>II^</b> complex with a shortened Pd—Cl bond induced by the bulky terpyridyl ligand 6,6''-dimesityl-2,2':6',2''-terpyridine
Onoda, Akira; Kawakita, Keiko; Okamura, Taka-aki; Yamamoto, Hitoshi; Ueyama, Norikazu; Acta Crystallographica Section E 59 (2003) m291–m293; doi:10.1107/S1600536803008626

data_2201985
_publ_section_title
;
 A distorted square-planar Pd^<b>II^</b> complex with a shortened
 Pd---Cl bond induced by the bulky terpyridyl ligand
 6,6''-dimesityl-2,2':6',2''-terpyridine
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m291
_journal_page_last               m293
_journal_paper_doi               10.1107/S1600536803008626
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd Cl (C33 H31 N3)]2 [Pd Cl4], 4 C H2 Cl2'
_chemical_formula_sum            'C70 H70 Cl14 N6 Pd3'
_chemical_formula_weight         1810.82
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.21
_cell_angle_beta                 100.468(7)
_cell_angle_gamma                83.566(7)
_cell_formula_units_Z            1
_cell_length_a                   10.6555(7)
_cell_length_b                   21.3398(5)
_cell_length_c                   8.59950(10)
_cell_measurement_reflns_used    12443
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.3
_cell_volume                     1910.75(14)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control
Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control
Software (Molecular Structure Corporation, 1991)
;
_computing_data_reduction
;
TEXSAN
(Molecular Structure Corporation, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Rigaku R-AXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.1689
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9543
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.531
_refine_diff_density_min         -1.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8029
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.078P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                4933
_reflns_number_total             8029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fl6020.cif
_cod_data_source_block           I
_cod_database_code               2201985