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_4112892
_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            'C50 H74 F12 N4 O21 P4 Pt2 S4'
_chemical_formula_weight         1937.43
_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                89.8587(7)
_cell_angle_beta                 88.1624(8)
_cell_angle_gamma                80.5377(16)
_cell_formula_units_Z            1
_cell_length_a                   8.8035(2)
_cell_length_b                   9.1015(2)
_cell_length_c                   23.3350(7)
_cell_measurement_reflns_used    5074
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     1843.32(8)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11961
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_correction_T_min  0.4280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinwski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       plate
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.887
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0028(4)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         8082
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+4.4478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                7006
_reflns_number_total             8082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0388919si20040709_024047_5.cif
_cod_data_source_block           complex8
_cod_database_code               4112892