Nanoporous lanthanide metal‒organic frameworks as efficient heterogeneous catalysts for the Henry reaction
Karmakar, Anirban; Hazra, Susanta; Guedes da Silva, M. Fátima C.; Paul, Anup; Pombeiro, Armando J. L.; CrystEngComm 18 (2016) 1337–; doi:10.1039/C5CE01456E

data_7223897
_publ_section_title
;
 Nanoporous lanthanide metal--organic frameworks as efficient
 heterogeneous catalysts for the Henry reaction
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1337
_journal_paper_doi               10.1039/C5CE01456E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C20 H14 N2 O10 Sm, C H4 N O, 2(C H3 N O)'
_chemical_formula_sum            'C23 H24 N5 O13 Sm'
_chemical_formula_weight         728.82
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-01-08 deposited with the CCDC.
2016-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   26.681(3)
_cell_length_b                   26.681(3)
_cell_length_c                   26.681(3)
_cell_measurement_reflns_used    7415
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.86
_cell_volume                     18994(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36111
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.307
_diffrn_reflns_theta_min         2.645
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       Block
_exptl_crystal_F_000             8712
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.101
_platon_squeeze_details
;
 The Platon SQUEEZE procedure was applied to recover 1520 electrons per
 unit cell in a void (total volume 8109 A^3), that is, 63 electrons
 per formula unit. On the basis of microanalytical data, the void content
 may include 1 protonated formamide and 2 formamide molecules, i.e.,
 a total of 73 electrons not far from the values estimated by SQUEEZE.
 Those solvent molecules have been included in the formula for the
 calculation of intensive  properties, thus justifying the checkcif
 report allerts CHEMW03_ALERT_2_A and DIFF003_ALERT_1_A. 
 PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2872
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0649P)^2^+198.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1951
_reflns_number_total             2872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01456e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7223893--7223897.cif.'
_cod_original_cell_volume        18993(7)
_cod_database_code               7223897
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.830
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              81289
_shelx_fab_checksum              44512