Macrocyclic and Lantern Complexes of Palladium(II) with Bis(amidopyridine) Ligands: Synthesis, Structure, and Host-Guest Chemistry
Nancy L. S. Yue; Dana J. Eisler; Michael C. Jennings; Richard J. Puddephatt; Inorganic Chemistry 43 (2004) 7671–7681; doi:10.1021/ic048893+

data_4327395
_publ_section_title
;
 Macrocyclic and Lantern Complexes of Palladium(II) with
 Bis(amidopyridine) Ligands: Synthesis, Structure, and Host-Guest
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7671
_journal_page_last               7681
_journal_paper_doi               10.1021/ic048893+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C84 H66 F9 N16 O16 Pd2'
_chemical_formula_weight         1939.33
_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                81.9070(10)
_cell_angle_beta                 88.5860(10)
_cell_angle_gamma                68.9470(10)
_cell_formula_units_Z            1
_cell_length_a                   12.9654(2)
_cell_length_b                   13.1454(2)
_cell_length_c                   15.8598(3)
_cell_measurement_temperature    200(2)
_cell_volume                     2496.53(7)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38843
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9469
_exptl_absorpt_correction_T_min  0.8501
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             983
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8512
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.425
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+4.5412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2158
_refine_ls_wR_factor_ref         0.2281
_reflns_number_gt                6707
_reflns_number_total             8512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488932Bsi20040811_112932_5.cif
_cod_data_source_block           3a
_cod_database_code               4327395