Circularly polarized luminescence induction on a Tb(III) complex with a tris(<i>o-tert</i>-butylaryloxide)-functionalized 1,4,7-triazacyclononane ligand coordinating chiral 1-phenylethylamine.
Shirai, Sora; Muratsugu, Satoshi; Matsui, Hisaki; Harada, Kazuhiro; Ehara, Masahiro; Nakai, Hidetaka; Tada, Mizuki; Chemical communications (Cambridge, England) 60 (2024) 14180–14183; doi:10.1039/d4cc05191b

data_7133875
_publ_section_title
;
 Circularly polarized luminescence induction on a Tb(III) complex with a
 tris(<i>o-tert</i>-butylaryloxide)-functionalized 1,4,7-triazacyclononane
 ligand coordinating chiral 1-phenylethylamine.
;
_journal_issue                   96
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14180
_journal_page_last               14183
_journal_paper_doi               10.1039/d4cc05191b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C15 H22.333 N1.333 O1.333 Tb0.333'
_chemical_formula_sum            'C15 H22.33 N1.33 O1.33 Tb0.33'
_chemical_formula_weight         295.65
_chemical_name_systematic        tBu1Tb
_chemical_properties_physical    Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   13.9426(3)
_cell_length_b                   13.9426(3)
_cell_length_c                   39.4010(12)
_cell_measurement_reflns_used    18402
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.4140
_cell_measurement_theta_min      2.6240
_cell_volume                     6633.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.850
_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    -87.00  50.00   0.50   73.35    --    1.60  45.00  90.00  274
  2  \w      3.00  35.00   0.50   73.35    --    1.60  45.00   0.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026758000
_diffrn_orient_matrix_UB_12      -0.0061553000
_diffrn_orient_matrix_UB_13      -0.0177640000
_diffrn_orient_matrix_UB_21      -0.0511114000
_diffrn_orient_matrix_UB_22      -0.0010937000
_diffrn_orient_matrix_UB_23      -0.0020163000
_diffrn_orient_matrix_UB_31      0.0289179000
_diffrn_orient_matrix_UB_32      0.0583526000
_diffrn_orient_matrix_UB_33      -0.0019404000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            17059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.202
_diffrn_reflns_theta_min         2.669
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             2772
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+9.2667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3840
_reflns_number_total             4086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05191b2.cif
_cod_data_source_block           230316_ss189_tbume1tb_02
_cod_depositor_comments
'Adding full bibliography for 7133875--7133876.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7133875
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C45H67N4O4Tb1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H17A-C17
 0.96 with sigma of 0.02
 H17B-C17
 0.96 with sigma of 0.02
 H17C-C17
 0.96 with sigma of 0.02
 H15-C15
 1 with sigma of 0.02
 H16A-C16
 0.96 with sigma of 0.02
 H16B-C16
 0.96 with sigma of 0.02
 H16C-C16
 0.96 with sigma of 0.02
 H17C-N2
 2.008 with sigma of 0.04
 H17A-N2
 2.008 with sigma of 0.04
 H17C-H17A
 1.568 with sigma of 0.04
 H17B-N2
 2.008 with sigma of 0.04
 H17A-H17B
 1.568 with sigma of 0.04
 H17B-H17C
 1.568 with sigma of 0.04
 H15-N2
 2 with sigma of 0.04
 H16A-H16B
 1.568 with sigma of 0.04
 H16B-H16C
 1.568 with sigma of 0.04
 H16C-H16A
 1.568 with sigma of 0.04
 H16A-N2
 2.008 with sigma of 0.04
 H16B-N2
 2.008 with sigma of 0.04
 H16C-N2
 2.008 with sigma of 0.04
3. Others
 Fixed Sof: C15(0.333333) C17(0.333333) H17A(0.333333) N2(0.333333)
 C16(0.333333) H15(0.333333) H17C(0.333333) H17B(0.333333) H16A(0.333333)
 H16B(0.333333) H16C(0.333333)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              67942
_shelx_hkl_checksum              25373
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.851