Modulation of pore shape and adsorption selectivity by ligand functionalization in a series of “rob”-like flexible metal‒organic frameworks
Cepeda, Javier; Pérez-Mendoza, Manuel; Calahorro, Antonio J.; Casati, Nicola; Seco, José Manuel; Aragones-Anglada, Marta; Moghadam, Peyman Z.; Fairen-Jimenez, David; Rodríguez-Diéguez, Antonio; Journal of Materials Chemistry A 6 (2018) 17409–; doi:10.1039/C8TA04316G

data_7237153
_publ_section_title
;
 Modulation of pore shape and adsorption selectivity by ligand
 functionalization in a series of &#x201C;rob&#x201D;-like flexible
 metal--organic frameworks
;
_journal_issue                   36
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              17409
_journal_paper_doi               10.1039/C8TA04316G
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C22 H20 Cu2 N4 O7, 4(H2 O)'
_chemical_formula_sum            'C22 H28 Cu2 N4 O13'
_chemical_formula_weight         683.56
_chemical_name_systematic
'poly-{[(mu-2,5-bis(4-pyridyl)-1,3,4-oxadiazole)-kN,N')bis(mu4-glutarato-kO:kO':kO'':kO''')dicopper(II)] tetrahydrate}'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.82(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9173(1)
_cell_length_b                   12.987(1)
_cell_length_c                   8.574(1)
_cell_measurement_reflns_used    34817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.767
_cell_measurement_theta_min      2.824
_cell_volume                     2897.5(4)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.767
_diffrn_reflns_theta_min         2.851
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1400
_exptl_crystal_preparation       adsorption
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
TITL shelx     C 2/c        R = 0.05
CELL   26.9173   12.9871    8.5739     90.00    104.82     90.00
SPGR C2/c
C101 0.046 0.411 0.839 !       1.03 eA-3
C102 1.001 0.498 0.163 !       0.91 eA-3
C103 0.525 0.048 0.344 !       0.86 eA-3
C104 0.984 0.466 0.716 !       0.84 eA-3
C105 0.538 0.015 0.880 !       0.83 eA-3
C106 0.986 0.451 0.409 !       0.80 eA-3
C107 0.953 0.420 0.154 !       0.80 eA-3
C108 0.525 0.076 0.907 !       0.79 eA-3
C109 0.448 0.078 0.475 !       0.78 eA-3
C110 0.468 0.118 0.429 !       0.78 eA-3
C111 0.405 0.097 0.975 !       0.77 eA-3
C112 0.513 0.064-0.010 !       0.76 eA-3
Q113 0.868 0.221 0.119 !       0.76 eA-3
C114 0.011 0.327 0.215 !       0.75 eA-3
C115 0.017 0.333 0.749 !       0.75 eA-3
C116 0.509 0.062 0.066 !       0.74 eA-3
C117 0.961 0.500 0.535 !       0.74 eA-3
C118 0.477 0.112 0.065 !       0.74 eA-3
C119 0.524 0.034 0.063 !       0.73 eA-3
C120 0.436 0.079 0.752 !       0.73 eA-3
Q121 0.758 0.365 0.814 !       0.73 eA-3
Q122 0.704 0.220 0.500 !       0.73 eA-3
C123 0.445 0.172 0.186 !       0.73 eA-3
C124 0.511 0.091 0.343 !       0.72 eA-3
C125 0.954 0.444 0.843 !       0.72 eA-3
C126 0.436 0.091 0.566 !       0.72 eA-3
Q127 0.352 0.338 0.688 !       0.71 eA-3
C128 0.981 0.618 0.247 !       0.71 eA-3
Q129 0.884 0.084 0.716 !       0.71 eA-3
C130 0.477 0.064-0.005 !       0.71 eA-3
C131 0.059 0.410 0.035 !       0.70 eA-3
C132 0.514 0.118 0.820 !       0.70 eA-3
C133 0.492 0.128 0.867 !       0.70 eA-3
C134 0.032 0.334 0.881 !       0.70 eA-3
C135 0.462 0.108 0.907 !       0.70 eA-3
Q136 0.772 0.484 0.783 !       0.69 eA-3
C137 0.930 0.342 0.606 !       0.69 eA-3
Q138 0.430 0.422 0.410 !       0.69 eA-3
C139 0.011 0.455 0.285 !       0.69 eA-3
C140 0.025 0.326 0.153 !       0.69 eA-3
Q141 0.414 0.424 0.165 !       0.69 eA-3
Q142 0.960 0.203 0.937 !       0.69 eA-3
C143 0.078 0.386 0.367 !       0.68 eA-3
C144 0.954 0.449 0.740 !       0.68 eA-3
C145 0.497 0.122-0.001 !       0.67 eA-3
C146 0.953 0.391 0.277 !       0.67 eA-3
Q147 0.142 0.253 0.064 !       0.67 eA-3
C148 0.530 0.124 0.179 !       0.66 eA-3
Q149 0.749 0.441 0.028 !       0.66 eA-3
Q150 0.368 0.078 0.221 !       0.65 eA-3
Q151 0.516 0.439 0.412 !       0.65 eA-3
Q152 0.907 0.345 0.882 !       0.65 eA-3
Q153 0.680 0.078 0.878 !       0.65 eA-3
Q154 0.711 0.184 0.431 !       0.65 eA-3
Q155 0.884 0.122 0.463 !       0.65 eA-3
Q156 0.726 0.484-0.006 !       0.65 eA-3
C157 0.586 0.079 0.147 !       0.65 eA-3
Q158 0.149 0.285 0.343 !       0.65 eA-3
Q159 0.752 0.296 0.843 !       0.64 eA-3
Q160 0.219 0.357 0.878 !       0.64 eA-3
Q161 0.843 0.271 0.253 !       0.64 eA-3
Q162 0.242 0.014 0.407 !       0.64 eA-3
Q163 0.734 0.061 0.030 !       0.64 eA-3
Q164 0.210 0.471 0.125 !       0.63 eA-3
Q165 0.649 0.343 0.689 !       0.63 eA-3
Q166 0.525 0.332 0.269 !       0.63 eA-3
Q167 0.757 0.183 0.276 !       0.63 eA-3
Q168 0.610 0.171 0.224 !       0.63 eA-3
Q169 0.711 0.107 0.064 !       0.63 eA-3
Q170 0.639 0.264 0.667 !       0.63 eA-3
C171 0.569 0.030 0.001 !       0.62 eA-3
Q172 0.842 0.311 0.037 !       0.62 eA-3
Q173 0.507 0.450 0.587 !       0.62 eA-3
C174 0.938 0.504 0.811 !       0.62 eA-3
Q175 0.758 0.441 0.658 !       0.62 eA-3
Q176 0.736 0.326 0.373 !       0.61 eA-3
Q177 0.602 0.061 0.432 !       0.61 eA-3
Q178 0.132 0.422 0.501 !       0.61 eA-3
C179 0.564 0.092 0.249 !       0.61 eA-3
C180 0.469 0.032 0.341 !       0.61 eA-3
Q181 0.150 0.097 0.248 !       0.61 eA-3
Q182 0.195 0.468 0.750 !       0.60 eA-3
Q183 0.986 0.155 0.277 !       0.60 eA-3
C184 0.094 0.433 0.471 !       0.60 eA-3
Q185 0.874 0.502 0.035 !       0.60 eA-3
Q186 0.766 0.065 0.874 !       0.60 eA-3
C187 0.430 0.070 0.061 !       0.60 eA-3
C188 0.464 0.173 0.032 !       0.60 eA-3
Q189 0.064 0.166 0.399 !       0.60 eA-3
Q190 0.212 0.035 0.896 !       0.59 eA-3
Q191 0.852 0.645 0.659 !       0.59 eA-3
Q192 0.352 0.145 0.659 !       0.59 eA-3
Q193 0.608 0.107 0.716 !       0.59 eA-3
Q194 0.378 0.358 0.276 !       0.59 eA-3
C195 0.437 0.014 0.417 !       0.59 eA-3
C196 0.008 0.510 0.478 !       0.59 eA-3
Q197 0.025 0.297 0.318 !       0.59 eA-3
Q198 0.406 0.139 0.566 !       0.59 eA-3
Q199 0.788 0.084 0.381 !       0.59 eA-3
;
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2743
_reflns_number_total             3755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta04316g2.cif
_cod_data_source_block           GR-MOF-5
_cod_original_cell_volume        2897.5(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7237153
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              9015
_shelx_hkl_checksum              38733
_shelx_fab_checksum              48462