Dynamic and Redox Active Pillared Bilayer Open Framework: Single-Crystal-to-Single-Crystal Transformations upon Guest Removal, Guest Exchange, and Framework Oxidation
Hye Jin Choi; Myunghyun Paik Suh; Journal of the American Chemical Society 126 (2004) 15844–15851; doi:10.1021/ja0466715

data_4113246
_publ_contact_author_address
'School of Chemistry, Seoul National University'
_publ_contact_author_email       mpsuh@snu.ac.kr
_publ_contact_author_fax         '+82 2 886 8516'
_publ_contact_author_name        'Myunghyun Paik Suh (Prof.)'
_publ_contact_author_phone       '+82 2 880 7760'
_publ_section_title
;
 Dynamic and Redox Active Pillared Bilayer Open Framework:
 Single-Crystal-to-Single-Crystal Transformations upon Guest Removal,
 Guest Exchange, and Framework Oxidation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15844
_journal_page_last               15851
_journal_paper_doi               10.1021/ja0466715
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C114 H202 I14 N30 Ni6 O41'
_chemical_formula_weight         4777.92
_chemical_name_systematic
;
  triclinic
;
_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                71.255(2)
_cell_angle_beta                 70.065(2)
_cell_angle_gamma                74.827(2)
_cell_formula_units_Z            1
_cell_length_a                   16.4340(14)
_cell_length_b                   19.9138(18)
_cell_length_c                   20.3375(18)
_cell_measurement_temperature    293(2)
_cell_volume                     5837.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_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  0.1936
_diffrn_reflns_av_sigmaI/netI    0.6030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38570
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    2.381
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             2334
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.0000(2)
_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   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         26977
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.4654
_refine_ls_R_factor_gt           0.1547
_refine_ls_shift/su_max          1.022
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3337
_refine_ls_wR_factor_ref         0.4960
_reflns_number_gt                5224
_reflns_number_total             26977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0466715si20040610_025223.cif
_cod_data_source_block           compound
_cod_database_code               4113246