Synthesis of macrocyclic salen rare-earth complexes and their framework conversion regulated by coordination sphere engineering.
Liu, Yi-Fu; Gil-Ramírez, Guzmán; Nakamura, Takashi; Chemical communications (Cambridge, England) 61 (2025) 921–924; doi:10.1039/d4cc03851g

data_7134001
_publ_section_title
;
 Synthesis of macrocyclic salen rare-earth complexes and their framework
 conversion regulated by coordination sphere engineering.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              921
_journal_page_last               924
_journal_paper_doi               10.1039/d4cc03851g
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'(C146 H172 F6 N16 O28 S2 Y4 2+), (C F3 S O3 -)2'
_chemical_formula_sum            'C148 H172 F12 N16 O34 S4 Y4'
_chemical_formula_weight         3430.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1914(19)
_cell_length_b                   31.770(6)
_cell_length_c                   32.931(6)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.841
_cell_measurement_theta_min      2.188
_cell_volume                     10662(3)
_computing_cell_refinement       'APEX3 (Bruker Nano, 2019)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'APEX3 (Bruker Nano, 2019)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2093
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            215219
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.250
_diffrn_reflns_theta_max         23.250
_diffrn_reflns_theta_min         1.237
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
TITL n597a_a          P 21 21 2    R = 0.17
CELL   10.1914   31.7700   32.9310     90.00     90.00     90.00
SPGR P21212
C101 0.554 0.982 0.961 !       5.90 eA-3
C102 0.046 0.727 0.187 !       4.76 eA-3
C103 0.368 0.008 0.993 !       4.40 eA-3
C104 0.969 0.440 0.031 !       3.89 eA-3
Q105 0.156 0.119 0.734 !       3.68 eA-3
C106 0.180 0.531 0.070 !       3.08 eA-3
Q107 0.661 0.506 0.145 !       3.07 eA-3
C108 0.178 0.725 0.209 !       3.01 eA-3
C109 0.388 0.993 0.923 !       2.99 eA-3
C110 0.066 0.006 0.633 !       2.83 eA-3
C111 0.569 0.530 0.859 !       2.68 eA-3
Q112 0.244 0.662 0.170 !       2.60 eA-3
C113 0.060 0.014 0.195 !       2.57 eA-3
C114 0.098 1.002 0.855 !       2.37 eA-3
C115 0.170 0.692 0.226 !       2.35 eA-3
C116 0.088 0.515 0.438 !       2.28 eA-3
C117 0.374 0.911 0.266 !       2.22 eA-3
C118 0.381 0.479 0.827 !       2.19 eA-3
C119 0.962 0.461 0.744 !       2.10 eA-3
C120 0.802 0.480 0.701 !       2.09 eA-3
C121 0.496 0.921 0.210 !       2.09 eA-3
C122 0.354 0.990 0.757 !       2.08 eA-3
C123 0.014 1.002 0.250 !       2.08 eA-3
Q124 0.145 0.013 0.639 !       2.08 eA-3
C125 0.325 0.259 0.772 !       2.08 eA-3
C126 0.563 0.924 0.195 !       2.05 eA-3
C127 0.548 0.014 0.749 !       2.04 eA-3
C128 0.868 0.485 0.259 !       2.04 eA-3
C129 0.052 0.469 0.289 !       2.00 eA-3
Q130 0.672 0.946 0.962 !       2.00 eA-3
C131 0.343 0.968 0.728 !       1.98 eA-3
C132 0.458 0.969 0.726 !       1.96 eA-3
Q133 0.629 0.351 0.173 !       1.95 eA-3
C134 0.387 0.030 0.264 !       1.94 eA-3
C135 0.458 0.945 0.236 !       1.94 eA-3
C136 0.034 0.974 0.203 !       1.94 eA-3
C137 0.244 0.989 0.643 !       1.92 eA-3
C138 0.547 0.977 0.759 !       1.89 eA-3
C139 0.082 0.468 0.329 !       1.88 eA-3
C140 0.046 0.115 0.740 !       1.87 eA-3
C141 0.035 0.469 0.258 !       1.87 eA-3
C142 0.944 0.484 0.227 !       1.82 eA-3
C143 0.599 0.952 0.297 !       1.82 eA-3
C144 0.943 0.470 0.265 !       1.82 eA-3
Q145 0.437 0.408 0.244 !       1.81 eA-3
C146 0.199 0.955 0.234 !       1.79 eA-3
C147 0.064 0.415 0.719 !       1.79 eA-3
C148 0.574 0.970 0.242 !       1.78 eA-3
C149 0.413 0.977 0.952 !       1.77 eA-3
C150 0.053 0.886 0.748 !       1.75 eA-3
C151 0.079 0.018 0.218 !       1.75 eA-3
C152 0.971 0.443 0.711 !       1.73 eA-3
C153 0.649 0.991 0.251 !       1.72 eA-3
C154 0.272 0.039 0.263 !       1.71 eA-3
C155 0.439 0.016 0.717 !       1.70 eA-3
C156 0.460 0.482 0.373 !       1.69 eA-3
Q157 0.244 0.388 0.452 !       1.69 eA-3
C158 0.857 0.014 0.640 !       1.69 eA-3
Q159 0.844 0.439 0.827 !       1.68 eA-3
C160 0.075 0.945 0.626 !       1.67 eA-3
C161 0.558 0.493 0.344 !       1.66 eA-3
C162 0.501 0.496 0.843 !       1.65 eA-3
Q163 0.119 0.453 0.843 !       1.63 eA-3
C164 0.830 0.945 0.250 !       1.63 eA-3
C165 0.608 0.554 0.805 !       1.62 eA-3
C166 0.506 0.946 0.764 !       1.62 eA-3
C167 0.468 0.469 0.821 !       1.60 eA-3
C168 0.620 0.469 0.713 !       1.59 eA-3
C169 0.083 0.466 0.695 !       1.59 eA-3
C170 0.946 0.453 0.814 !       1.59 eA-3
C171 0.449 0.501 0.734 !       1.58 eA-3
C172 0.556 0.031 0.258 !       1.58 eA-3
C173 1.011 0.516 0.319 !       1.57 eA-3
Q174 0.344 0.390 0.250 !       1.55 eA-3
C175 0.299 0.961 0.196 !       1.54 eA-3
C176 0.218 0.938 0.213 !       1.54 eA-3
Q177 0.865 0.436 0.726 !       1.54 eA-3
Q178 0.846 0.360 0.376 !       1.53 eA-3
Q179 0.743 0.300 0.171 !       1.53 eA-3
Q180 1.014 0.516 0.429 !       1.52 eA-3
Q181 0.159 0.493 0.455 !       1.51 eA-3
C182 0.531 0.484 0.696 !       1.51 eA-3
C183 0.976 0.485 0.719 !       1.51 eA-3
C184 0.509 0.500 0.868 !       1.51 eA-3
C185 0.271 0.452 0.805 !       1.51 eA-3
C186 0.705 0.456 0.711 !       1.49 eA-3
C187 0.148 0.961 0.235 !       1.47 eA-3
C188 0.740 0.967 0.234 !       1.47 eA-3
C189 0.122 0.444 0.774 !       1.47 eA-3
Q190 0.139 0.883 0.759 !       1.46 eA-3
C191 0.742 0.049 0.236 !       1.46 eA-3
Q192 0.151 0.139 0.616 !       1.46 eA-3
Q193 0.356 0.382 0.275 !       1.44 eA-3
C194 0.193 0.476 0.321 !       1.42 eA-3
Q195 0.903 0.016 0.603 !       1.41 eA-3
Q196 0.344 0.381 0.312 !       1.41 eA-3
Q197 0.152 0.640 0.195 !       1.40 eA-3
C198 0.917 0.046 0.273 !       1.40 eA-3
Q199 0.344 0.462 0.701 !       1.40 eA-3
;
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 3348 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(5)
_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     1042
_refine_ls_number_reflns         15303
_refine_ls_number_restraints     425
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1053
_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^)+(0.1690P)^2^+33.9215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2676
_refine_ls_wR_factor_ref         0.2968
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10981
_reflns_number_total             15303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03851g2.cif
_cod_data_source_block           n597a_a_sq
_cod_depositor_comments
'Adding full bibliography for 7134001--7134003.cif.'
_cod_database_code               7134001
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.537
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              10089
_shelx_hkl_checksum              23218
_shelx_fab_checksum              47195
_platon_squeeze_void_probe_radius 1.20