Self-Assembly of a Pd6-Molecular Double-Square and a Cu3-Trigonalbipyramidal Cage via a New Tripodal Flexible Ligand
Arun Kumar Bar; Rajesh Chakrabarty; Partha Sarathi Mukherjee; Inorganic Chemistry 48 (2009) 10880–10882; doi:10.1021/ic901633g

data_4303724
_publ_section_title
;
Self-Assembly of a Pd6-Molecular Double-Square and a
Cu3-Trigonalbipyramidal Cage via a New Tripodal Flexible Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10880
_journal_page_last               10882
_journal_paper_doi               10.1021/ic901633g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C144 H240 N36 Pd6, 8(Cl O4), 4(N O3)'
_chemical_formula_sum            'C144 H240 Cl8 N40 O44 Pd6'
_chemical_formula_weight         4157.83
_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                105.75(3)
_cell_angle_beta                 101.71(3)
_cell_angle_gamma                93.90(3)
_cell_formula_units_Z            6
_cell_length_a                   16.057(3)
_cell_length_b                   18.914(4)
_cell_length_c                   22.570(5)
_cell_measurement_temperature    150(2)
_cell_volume                     6405(3)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BR5UKER SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.818
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15500
_diffrn_reflns_theta_full        23.51
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.9313
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   emperical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'color less'
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
contributions.  Total electron count found = 472/unit cell.
Calculated for 15 nitromethane (the reaction solvent)
= 480/unit cell.  The intensive properties (density, F(000), etc.)
reflect these contributions
;
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         15500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.391
_refine_ls_shift/su_mean         0.076
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3021
_refine_ls_wR_factor_ref         0.3147
_reflns_number_gt                12801
_reflns_number_total             9344
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic901633g_si_002.cif
_cod_data_source_block           complex-1
_cod_original_cell_volume        6404(2)
_cod_original_formula_sum        'C144 H240 N40 O44 Cl8 Pd6'
_cod_database_code               4303724