Stepwise selective crystallization of Fe and Dy complexes from a Fe/Nd/Dy mixture: separation despite charge and solubility similarity.
Hasegawa, Natsuki; Yanai, Akiho; Masaki, Hinako; Kirishima, Akira; Tsunashima, Ryo; Masuya-Suzuki, Atsuko; Chemical communications (Cambridge, England) 61 (2025) 17384–17387; doi:10.1039/d5cc03074a

data_7135045
_publ_section_title
;
 Stepwise selective crystallization of Fe and Dy complexes from a Fe/Nd/Dy
 mixture: separation despite charge and solubility similarity.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17384
_journal_page_last               17387
_journal_paper_doi               10.1039/d5cc03074a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C27 H27 Dy N4 O3'
_chemical_formula_weight         618.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2025-05-30 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.375(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7777(16)
_cell_length_b                   19.0804(16)
_cell_length_c                   7.7909(6)
_cell_measurement_reflns_used    4245
_cell_measurement_temperature    223
_cell_measurement_theta_max      29.0240
_cell_measurement_theta_min      2.1230
_cell_volume                     2473.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1335
_diffrn_reflns_av_unetI/netI     0.1309
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.135
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.00055(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3487
_reflns_number_total             5613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03074a2.cif
_cod_data_source_block           exp_1230_auto
_cod_depositor_comments          'Adding full bibliography for 7135045.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7135045
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.711
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              39754
_shelx_hkl_checksum              54340