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_4121781
_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            'C79 H93 N9 O16 Zn2'
_chemical_formula_weight         1555.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.568(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.336(3)
_cell_length_b                   23.766(4)
_cell_length_c                   15.808(3)
_cell_measurement_reflns_used    166
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     7853(2)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_unetI/netI     0.1873
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35776
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         2.595
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6402
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
 The unit cell was calculated to contain an estimated 
 8 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         0.962
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2429 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         13360
_refine_ls_number_restraints     1004
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1185P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2551
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7688
_reflns_number_total             13360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502238a_si_003.cif
_cod_data_source_block           kz118_sq_s
_cod_depositor_comments
'Adding full bibliography for 4121779--4121781.cif.'
_cod_database_code               4121781
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.947