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_4105593
_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_moiety
;
C72 H96 N18 O18 Pd3, 3(C3 H6 O), 6(B F4), H2 O
;
_chemical_formula_sum            'C81 H116 B6 F24 N18 O22 Pd3'
_chemical_formula_weight         2533.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
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_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                   15.5209(6)
_cell_length_b                   15.5209(6)
_cell_length_c                   39.8268(18)
_cell_measurement_reflns_used    5929
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      2.55
_cell_volume                     8308.8(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            15285
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.8421
_exptl_absorpt_correction_T_min  0.7362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       triangle
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+0.1703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                5071
_reflns_number_total             6243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1093925_si_002.cif
_cod_data_source_block           nth
_cod_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4105593