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_7720065
_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 H39 La N4 O6, 2(Cl O4)'
_chemical_formula_sum            'C32 H39 Cl2 La N4 O14'
_chemical_formula_weight         913.48
_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
_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                 109.809(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3932(4)
_cell_length_b                   11.4737(2)
_cell_length_c                   16.2053(4)
_cell_measurement_reflns_used    6520
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      73.4430
_cell_measurement_theta_min      4.4690
_cell_volume                     3567.43(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_temperature      173.00
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
  1 omega  -79.00  -14.00   1.0000    3.3100
omega____ theta____ kappa____ phi______ frames
    -      -42.3568  -57.0000  150.0000 65

  2 omega -117.00  -18.00   1.0000    3.3100
omega____ theta____ kappa____ phi______ frames
    -      -42.3568  -38.0000    0.0000 99

  3 omega    2.00   77.00   1.0000    3.3100
omega____ theta____ kappa____ phi______ frames
    -       42.3568 -125.0000  -60.0000 75

  4 omega   45.00  129.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513  -77.0000 -120.0000 84

  5 omega   77.00  103.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   61.0000 -180.0000 26

  6 omega  111.00  174.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000 -180.0000 63

  7 omega   77.00  105.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   61.0000 -150.0000 28

  8 omega   78.00  171.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   61.0000 -120.0000 93

  9 omega   73.00   99.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000 -180.0000 26

 10 omega   73.00   99.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000 -150.0000 26

 11 omega   74.00  164.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513  125.0000  -30.0000 90

 12 omega   74.00  171.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000  120.0000 97

 13 omega  103.00  167.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000  150.0000 64

 14 omega   73.00   98.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513   77.0000  150.0000 25

 15 omega   41.00   86.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513 -125.0000  120.0000 45

 16 omega   33.00   58.00   1.0000    5.1600
omega____ theta____ kappa____ phi______ frames
    -      105.7513  -30.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21197
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.696
_diffrn_reflns_theta_min         4.490
_exptl_absorpt_coefficient_mu    11.283
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.161
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.2562
_exptl_crystal_size_mid          0.2059
_exptl_crystal_size_min          0.0689
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6886
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+2.3156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5382
_reflns_number_total             6886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03015c2.cif
_cod_data_source_block           La-KHQ-2ClO4
_cod_depositor_comments
'Adding full bibliography for 7720064--7720065.cif.'
_cod_original_cell_volume        3567.43(14)
_cod_database_code               7720065
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.510
_shelx_estimated_absorpt_t_min   0.160
_olex2_refinement_description
;
1. Restrained distances
 O8-H8
 0.9 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,
 H28B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B),
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C19(H19),
 C20(H20), C21(H21)
;
_shelx_res_checksum              98688
_olex2_submission_special_instructions 'No special instructions were received'