Hydroxyquinoline-functionalised aza-crown macrocycles for lanthanide coordination.
Siakalli, Christina; Osborne, Bradley E.; Brown, Ryan K.; Rocco, Claudia; Weiss, Dominik; García-España, Enrique V; Grundler, Pascal V.; Moiseeva, Anzhelika N.; Talip, Zeynep; van der Meulen, Nicholas P.; Ma, Michelle T.; Long, Nicholas J.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3413–3421; doi:10.1039/d5dt03015c

data_7720064
_publ_section_title
;
 Hydroxyquinoline-functionalised aza-crown macrocycles for lanthanide
 coordination.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3413
_journal_page_last               3421
_journal_paper_doi               10.1039/d5dt03015c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C32 H42 N4 O6, 2(Cl O4)'
_chemical_formula_sum            'C32 H42 Cl2 N4 O14'
_chemical_formula_weight         777.59
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-28 deposited with the CCDC.	2026-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.310(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2238(4)
_cell_length_b                   14.4135(6)
_cell_length_c                   12.2816(5)
_cell_measurement_reflns_used    3373
_cell_measurement_temperature    173(3)
_cell_measurement_theta_max      72.2610
_cell_measurement_theta_min      4.3890
_cell_volume                     1774.68(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  25.00   1.00    1.00    --  -42.36  57.00 -60.00   90
  2  \w      2.00  86.00   1.00    1.00    --   42.36-125.00  90.00   84
  3  \w     35.00 132.00   1.00    4.47    --  105.75 -45.00 120.00   97
  4  \w     54.00 170.00   1.00    4.47    --  105.75  15.00  30.00  116
  5  \w    150.00 178.00   1.00    4.47    --  105.75  77.00 150.00   28
  6  \w     73.00  99.00   1.00    4.47    --  105.75  77.00 150.00   26
  7  \w     77.00 170.00   1.00    4.47    --  105.75  61.00 150.00   93
  8  \w     77.00 177.00   1.00    4.47    --  105.75  61.00  60.00  100
  9  \w    126.00 176.00   1.00    4.47    --  105.75  61.00-150.00   50
 10  \w    127.00 153.00   1.00    4.47    --  105.75  77.00-180.00   26
 11  \w     77.00 168.00   1.00    4.47    --  105.75  30.00 -90.00   91
 12  \w     78.00 118.00   1.00    4.47    --  105.75  61.00-150.00   40
 13  \w     73.00  98.00   1.00    4.47    --  105.75  77.00-180.00   25
 14  \w   -115.00 -19.00   1.00    1.00    --  -42.36 -57.00 150.00   96
 15  \w   -110.00 -42.00   1.00    1.00    --  -42.36 -38.00-150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0776828000
_diffrn_orient_matrix_UB_12      -0.0543592000
_diffrn_orient_matrix_UB_13      -0.0747910000
_diffrn_orient_matrix_UB_21      -0.1326061000
_diffrn_orient_matrix_UB_22      -0.0320357000
_diffrn_orient_matrix_UB_23      -0.0727227000
_diffrn_orient_matrix_UB_31      -0.0002109000
_diffrn_orient_matrix_UB_32      0.0862338000
_diffrn_orient_matrix_UB_33      -0.0740604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11296
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.611
_diffrn_reflns_theta_min         4.410
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.553
_exptl_crystal_size_mid          0.442
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0666P)^2^+0.5469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2644
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03015c2.cif
_cod_data_source_block           KHQ-H2-2ClO4
_cod_depositor_comments
'Adding full bibliography for 7720064--7720065.cif.'
_cod_database_code               7720064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H38 Cl N4 O10 Tb'
_chemical_oxdiff_usercomment     CS52_TbkQOH
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C20(H20A,H20B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              88686
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.556
_oxdiff_exptl_absorpt_empirical_full_min 0.767