Self-Assembly of Flexible Supramolecular Metallacyclic Ensembles: Structures and Adsorption Properties of Their Nanoporous Crystalline Frameworks
Biswaroop Chatterjee; Juan C. Noveron; Marino J. E. Resendiz; Jie Liu; Takuya Yamamoto; Daniel Parker; Martin Cinke; Cattien V. Nguyen; Atta M. Arif; Peter J. Stang; Journal of the American Chemical Society 126 (2004) 10645–10656; doi:10.1021/ja0388919

data_4112890
_publ_section_title
;
 Self-Assembly of Flexible Supramolecular Metallacyclic Ensembles:
 Structures and Adsorption Properties of Their Nanoporous Crystalline
 Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10645
_journal_page_last               10656
_journal_paper_doi               10.1021/ja0388919
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C90 H92 F12 N4 O24 P4 Pd2 S4'
_chemical_formula_weight         2306.60
_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                91.9466(10)
_cell_angle_beta                 104.8438(12)
_cell_angle_gamma                90.2628(20)
_cell_formula_units_Z            1
_cell_length_a                   10.5043(2)
_cell_length_b                   12.0394(3)
_cell_length_c                   20.2334(6)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2471.77(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.1041
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12126
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.8384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         9915
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0351P)^2^+4.2099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7152
_reflns_number_total             9915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0388919si20040709_024047_3.cif
_cod_data_source_block           complex6
_cod_database_code               4112890