Metal-Organic Frameworks with Mechanically Interlocked Pillars: Controlling Ring Dynamics in the Solid-State via a Reversible Phase Change.
Zhu, Kelong; Vukotic, V. Nicholas; O'Keefe, Christopher A; Schurko, Robert W.; Loeb, Stephen J.; Journal of the American Chemical Society 136 (2014) 7403–7409; doi:10.1021/ja502238a

data_4121780
_publ_section_title
;
 Metal-Organic Frameworks with Mechanically Interlocked Pillars:
 Controlling Ring Dynamics in the Solid-State via a Reversible Phase
 Change.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7403
_journal_page_last               7409
_journal_paper_doi               10.1021/ja502238a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C112 H170 N16 O17 Zn2'
_chemical_formula_weight         2143.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.870(16)
_cell_length_b                   22.960(15)
_cell_length_c                   48.42(4)
_cell_measurement_temperature    150(2)
_cell_volume                     21942(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            203396
_diffrn_reflns_theta_full        70.18
_diffrn_reflns_theta_max         70.18
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.8963
_exptl_absorpt_correction_T_min  0.7596
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9200
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; The unit cell was calculated to contain an estimated  
  104 molecules of DMF which were treated as a diffuse contribution
  to the overall scattering without specific atom positions
  by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.765
_refine_diff_density_min         -2.368
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.37(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1465
_refine_ls_number_reflns         33929
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3056
_reflns_number_gt                27599
_reflns_number_total             33929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja502238a_si_004.cif
_cod_data_source_block           um1-non
_cod_depositor_comments
'Adding full bibliography for 4121779--4121781.cif.'
_cod_original_cell_volume        21942(31)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4121780