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_7223895
_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 La N2 O10, C3 H8 N O, 3(C3 H7 N O)'
_chemical_formula_sum            'C31 H43 La N6 O14'
_chemical_formula_weight         862.62
_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                   27.0059(7)
_cell_length_b                   27.0059(7)
_cell_length_c                   27.0059(7)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.82
_cell_volume                     19695.9(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0634
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50931
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.648
_diffrn_reflns_theta_min         2.613
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.384
_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    1.745
_exptl_crystal_description       Block
_exptl_crystal_F_000             10560
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.118
_platon_squeeze_details
;
 The Platon SQUEEZE procedure was applied to recover 4391 electrons per
 unit cell in a void (total volume 8336 A^3), that is, 183 electrons
 per formula unit. On the basis of microanalytical data, the void content
 may include 1 protonated dmf molecule as well as 3 dmf molecule,
 i.e., a total of 161 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         2.301
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3126
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1333P)^2^+283.6773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2390
_reflns_number_total             3126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01456e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7223893--7223897.cif.'
_cod_original_cell_volume        19695.9(15)
_cod_database_code               7223895
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.854
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              16713
_shelx_fab_checksum              99779