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_4112894
_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            'C98 H88 F12 N8 O24 P4 Pd2 S4'
_chemical_formula_weight         2454.68
_chemical_name_systematic
;
 ?
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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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                88.4998(8)
_cell_angle_beta                 81.9321(8)
_cell_angle_gamma                70.4728(13)
_cell_formula_units_Z            1
_cell_length_a                   11.7834(2)
_cell_length_b                   15.3708(3)
_cell_length_c                   15.4053(3)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2603.06(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19254
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.8215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         11811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0562P)^2^+6.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                8531
_reflns_number_total             11811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0388919si20040709_024047_7.cif
_cod_data_source_block           complex10
_cod_original_cell_volume        2603.06(8)
_cod_database_code               4112894