Lanthanide‒EDTA complexes covalently bonded on Fe3O4@SiO2 magnetic nanoparticles promote the green, stereoselective synthesis of N-acylhydrazones
de Resende Filho, João Batista M.; Falcão, Nathália Kellyne S. M.; Pires, Gilvan P.; de Vasconcelos, Luiz Fernando S.; Pinheiro, Sávio M.; dos Santos Filho, José Maurício; Frazão Barbosa, Marília Imaculada; Doriguetto, Antônio Carlos; Teotonio, Ercules E. S.; Vale, Juliana A.; New Journal of Chemistry 43 (2019) 14257–; doi:10.1039/C9NJ02916H

data_7058719
_publ_section_title
;
 Lanthanide--EDTA complexes covalently bonded on Fe3O4@SiO2 magnetic
 nanoparticles promote the green, stereoselective synthesis of
 N-acylhydrazones
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14257
_journal_paper_doi               10.1039/C9NJ02916H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C21 H18 Fe N4 O2'
_chemical_formula_sum            'C21 H18 Fe N4 O2'
_chemical_formula_weight         414.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-07-30 deposited with the CCDC.    2019-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.016(16)
_cell_length_b                   12.875(8)
_cell_length_c                   7.696(5)
_cell_measurement_reflns_used    4325
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      1.582
_cell_volume                     1884(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.813
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.813
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4325
_diffrn_reflns_point_group_measured_fraction_full 0.727
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         1.582
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan (SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 461 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.31(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2490
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+1.7179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.2004
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.624
_reflns_Friedel_fraction_max     0.617
_reflns_number_gt                1557
_reflns_number_total             2490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02916h2.cif
_cod_data_source_block           compound_14
_cod_depositor_comments          'Adding full bibliography for 7058719.cif.'
_cod_database_code               7058719
_shelxl_version_number           2014-3
_shelx_res_checksum              21977