Motion of an Isolated Water Molecule within a Flexible Coordination Cage: Structural Properties and Catalytic Effects of Ionic Palladium(II) Complexes
Tae Hwan Noh; Eunjung Heo; Kang Hyun Park; Ok-Sang Jung; Journal of the American Chemical Society 133 (2011) 1236–1239; doi:10.1021/ja1093925

data_4105594
_publ_section_title
;
 Motion of an Isolated Water Molecule within a Flexible Coordination Cage:
 Structural Properties and Catalytic Effects of Ionic Palladium(II)
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1236
_journal_page_last               1239
_journal_paper_doi               10.1021/ja1093925
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C81 H116 Cl6 N18 O47 Pd3'
_chemical_formula_weight         2625.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.52570(10)
_cell_length_b                   15.52570(10)
_cell_length_c                   40.6727(7)
_cell_measurement_reflns_used    3785
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.74
_cell_measurement_theta_min      2.51
_cell_volume                     8490.55(17)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            15732
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.8714
_exptl_absorpt_correction_T_min  0.7649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.732
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                3361
_reflns_number_total             6767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1093925_si_003.cif
_cod_data_source_block           th3
_cod_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4105594