Incorporation of an A1/A2-Difunctionalized Pillar[5]arene into a Metal-Organic Framework
Nathan L. Strutt; David Fairen-Jimenez; Julien Iehl; Marianne B. Lalonde; Randall Q. Snurr; Omar K. Farha; Joseph T. Hupp; J. Fraser Stoddart; Journal of the American Chemical Society 134 (2012) 17436–17439; doi:10.1021/ja3082523

data_4118824
_publ_section_title
;
 Incorporation of an A1/A2-Difunctionalized Pillar[5]arene into a
 Metal-Organic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17436
_journal_page_last               17439
_journal_paper_doi               10.1021/ja3082523
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C43 H46 O10'
_chemical_formula_weight         722.80
_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                 99.5880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2730(3)
_cell_length_b                   11.9713(2)
_cell_length_c                   17.7886(2)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      134.213
_cell_measurement_theta_min      8.431
_cell_volume                     4466.86(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0949
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24167
_diffrn_reflns_theta_full        67.62
_diffrn_reflns_theta_max         67.62
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.8760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Diffuse, disordered solvent molecules could not be adequately modeled.  The
bypass procedure in Platon (Spek, 1990) was used to remove the electronic
contribution from these solvents. The total potential solvent accessible void 
volume was 509 Ang^3^ and the electron count / cell = 187. As the exact solvent
content is not known, the reported formula reflects only the atoms used in the 
refinement.
;
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_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          0.2009
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                7331
_reflns_number_total             7579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3082523_si_002.cif
_cod_data_source_block           n1393_0m
_cod_database_code               4118824