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_7134002
_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         '(C144 H176 N16 O24 Lu4 4+), (C F3 S O3 -)4'
_chemical_formula_sum            'C148 H176 F12 Lu4 N16 O36 S4'
_chemical_formula_weight         3811.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 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                   10.4748(6)
_cell_length_b                   31.6860(15)
_cell_length_c                   32.6723(16)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.302
_cell_measurement_theta_min      2.398
_cell_volume                     10844.1(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1490
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            138748
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.374
_diffrn_reflns_theta_min         1.791
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6485
_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    1.167
_exptl_crystal_description       'triangle plate'
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
TITL n608c_a          I 2 2 2      R = 0.09
CELL   10.4748   31.6860   32.6723     90.00     90.00     90.00
SPGR I222
C101 0.657 0.492 0.017 !       3.28 eA-3
C102 0.501 0.476 0.000 !       2.94 eA-3
C103 0.371 0.383 0.491 !       2.69 eA-3
C104 0.406 0.494 0.009 !       2.63 eA-3
C105 0.081 0.978 0.468 !       2.56 eA-3
C106 0.712 0.404 0.453 !       2.29 eA-3
C107 0.166 0.977 0.492 !       2.25 eA-3
C108 0.100 0.065 0.100 !       2.21 eA-3
C109 0.128 0.501-0.001 !       2.16 eA-3
Q110 0.292 0.596 0.275 !       2.10 eA-3
C111 0.163 0.084 0.100 !       2.10 eA-3
Q112 0.191 0.360 0.367 !       2.06 eA-3
C113 0.306 0.461 0.035 !       2.02 eA-3
C114 0.551 0.514 0.383 !       2.02 eA-3
C115 0.254 0.501-0.001 !       1.93 eA-3
C116 1.003 0.501-0.002 !       1.89 eA-3
C117 0.496 0.498 0.046 !       1.88 eA-3
C118 1.000 0.475 0.001 !       1.86 eA-3
Q119 0.374 0.794 0.023 !       1.82 eA-3
C120 0.055 0.532 0.407 !       1.80 eA-3
C121 0.325 0.555 0.406 !       1.76 eA-3
Q122 0.202 0.572 0.382 !       1.76 eA-3
C123 0.028 0.484 0.062 !       1.71 eA-3
C124 0.461 0.461 0.478 !       1.70 eA-3
C125 0.156 0.563 0.427 !       1.70 eA-3
C126 0.434 0.373 0.493 !       1.69 eA-3
Q127 0.188 0.907 0.495 !       1.69 eA-3
C128 0.778 0.459 0.460 !       1.67 eA-3
Q129 0.387 0.351 0.367 !       1.67 eA-3
Q130 0.105 0.586 0.383 !       1.67 eA-3
C131 0.237 0.988 0.461 !       1.65 eA-3
Q132 0.522 0.937 0.468 !       1.63 eA-3
C133 0.942 0.481 0.000 !       1.63 eA-3
C134 0.729 0.876 0.071 !       1.62 eA-3
C135 0.594 0.964 0.491 !       1.62 eA-3
Q136 0.427 0.960 0.459 !       1.62 eA-3
C137 0.020 0.470 0.025 !       1.60 eA-3
C138 0.907 0.978 0.453 !       1.58 eA-3
C139 0.508 0.993 0.001 !       1.57 eA-3
C140 0.232 0.570 0.415 !       1.57 eA-3
C141 0.796 0.400 0.429 !       1.56 eA-3
C142 0.378 0.985 0.469 !       1.55 eA-3
C143 0.751 0.399 0.408 !       1.54 eA-3
C144 0.798 0.899 0.000 !       1.54 eA-3
C145 0.857 0.462 0.001 !       1.53 eA-3
C146 0.529 0.477 0.374 !       1.52 eA-3
C147 0.745 0.507 0.400 !       1.51 eA-3
C148 0.899 0.882 0.054 !       1.50 eA-3
C149 0.503 1.001 0.468 !       1.50 eA-3
Q150 0.212 0.221 0.079 !       1.49 eA-3
C151 0.895 0.866 0.040 !       1.48 eA-3
C152 0.715 0.497 0.606 !       1.47 eA-3
Q153 0.578 0.888 0.048 !       1.47 eA-3
C154 0.892 0.522 0.328 !       1.47 eA-3
C155 0.872 0.387 0.397 !       1.45 eA-3
C156 0.932 0.485 0.063 !       1.43 eA-3
C157 0.151 0.532 0.406 !       1.42 eA-3
C158 0.410 0.056 0.079 !       1.40 eA-3
C159 0.435 0.997 0.007 !       1.39 eA-3
C160 0.363 0.033 0.055 !       1.39 eA-3
C161 0.806 0.516 0.381 !       1.38 eA-3
C162 0.647 0.506 0.397 !       1.38 eA-3
C163 0.465 0.467 0.065 !       1.36 eA-3
C164 0.183 0.492 0.071 !       1.36 eA-3
Q165 0.427 0.798 0.025 !       1.36 eA-3
Q166 0.659 0.311 0.422 !       1.36 eA-3
C167 0.659 0.867 0.023 !       1.36 eA-3
C168 0.883 0.460 0.037 !       1.34 eA-3
C169 0.911 0.471 0.025 !       1.34 eA-3
C170 0.186 0.992 0.007 !       1.34 eA-3
Q171 0.625 0.012 0.186 !       1.33 eA-3
Q172 0.616 0.876 0.072 !       1.32 eA-3
C173 0.404 0.448 0.041 !       1.32 eA-3
Q174 0.089 0.318 0.490 !       1.31 eA-3
C175 0.943 0.480 0.484 !       1.31 eA-3
C176 0.637 0.015 0.101 !       1.30 eA-3
C177 0.257 0.857 0.002 !       1.29 eA-3
Q178 0.289 0.960 0.453 !       1.27 eA-3
Q179 0.769 0.336 0.470 !       1.25 eA-3
C180 0.818 0.990 0.452 !       1.25 eA-3
Q181 0.286 0.875 0.116 !       1.25 eA-3
Q182 0.409 0.447 0.078 !       1.23 eA-3
C183 0.547 0.962 0.452 !       1.23 eA-3
Q184 0.876 0.038 0.115 !       1.22 eA-3
C185 0.053 0.985 0.422 !       1.22 eA-3
Q186 0.340 0.834 0.000 !       1.22 eA-3
C187 0.008 0.359 0.493 !       1.22 eA-3
C188 0.140 0.368 0.491 !       1.20 eA-3
Q189 0.748 0.339 0.414 !       1.20 eA-3
Q190 0.214 0.468 0.070 !       1.20 eA-3
Q191 0.901 0.506 0.112 !       1.20 eA-3
Q192 0.979 0.307 0.459 !       1.20 eA-3
Q193 0.475 0.827 0.024 !       1.19 eA-3
C194 0.453 0.010 0.421 !       1.19 eA-3
C195 0.916 0.390 0.484 !       1.19 eA-3
C196 0.704 0.007 0.133 !       1.18 eA-3
C197 0.669 0.994 0.470 !       1.18 eA-3
C198 0.149 0.501 0.447 !       1.18 eA-3
C199 0.994 0.366 0.515 !       1.18 eA-3
;
_refine_diff_density_max         1.806
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 2768 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.060(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11116
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      5.375
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1214P)^2^+30.7300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7775
_reflns_number_total             11116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03851g2.cif
_cod_data_source_block           n608c_a_sq
_cod_depositor_comments
'Adding full bibliography for 7134001--7134003.cif.'
_cod_database_code               7134002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.554
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              54018
_shelx_hkl_checksum              22368
_shelx_fab_checksum              89016
_platon_squeeze_void_probe_radius 1.20