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_7237152
_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         'C24 H26 Cu2 N4 O8, 5(H2 O)'
_chemical_formula_sum            'C24 H36 Cu2 N4 O13'
_chemical_formula_weight         715.64
_chemical_name_systematic
'poly-{[(mu-1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene)-kN,N')bis(mu4-2-methylglutarato-kO:kO':kO'':kO''')dicopper(II)] pentahydrate}'
_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                 94.792(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.019(9)
_cell_length_b                   13.506(5)
_cell_length_c                   8.921(5)
_cell_measurement_reflns_used    25819
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.338
_cell_measurement_theta_min      2.34
_cell_volume                     3244(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0721
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25819
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.350
_diffrn_reflns_theta_max         23.338
_diffrn_reflns_theta_min         2.725
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.824
_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    1.465
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1480
_exptl_crystal_preparation       adsorption
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL shelx     C 2/c        R = 0.05
CELL   27.0190   13.5060    8.9210     90.00     94.79     90.00
SPGR C2/c
Q101 0.131 0.502 0.112 !       1.45 eA-3
Q102 0.907 0.406 0.059 !       0.83 eA-3
Q103 0.538 0.096 0.034 !       0.82 eA-3
Q104 0.952 0.437-0.003 !       0.79 eA-3
Q105 0.445 0.096 0.130 !       0.69 eA-3
Q106 0.450 0.043 0.282 !       0.54 eA-3
Q107 0.431 0.037 0.256 !       0.53 eA-3
Q108 0.023 0.230 0.075 !       0.51 eA-3
Q109 0.578 0.235 0.840 !       0.50 eA-3
;
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+20.5172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1893
_reflns_number_total             2337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta04316g2.cif
_cod_data_source_block           GR-MOF-3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7237152
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              59981
_shelx_hkl_checksum              59138
_shelx_fab_checksum              77714