Circularly polarized luminescence from Tb(III) interacting with chiral polyether macrocycles
Homberg, Alexandre; Navazio, Federica; Le Tellier, Antoine; Zinna, Francesco; Fürstenberg, Alexandre; Besnard, Céline; Di Bari, Lorenzo; Lacour, Jerome; Dalton Transactions  (2022) –; doi:10.1039/D2DT02627A

data_7711388
_publ_section_title
;
 Circularly polarized luminescence from Tb(III) interacting with chiral
 polyether macrocycles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02627A
_journal_year                    2022
_chemical_formula_moiety         'C48 H46 La N2 O10, 3(Cl O4), 4(C2 H3 N)'
_chemical_formula_sum            'C56 H58 Cl3 La N6 O22'
_chemical_formula_weight         1412.34
_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             2020-05-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-07-11 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5672(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5523(2)
_cell_length_b                   11.12589(12)
_cell_length_c                   23.3538(2)
_cell_measurement_reflns_used    38923
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      73.9580
_cell_measurement_theta_min      2.0730
_cell_volume                     6034.52(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -42.00 -13.00   0.50    2.00    --  -52.43 125.00-120.00   58
  2  \w    -81.00 -35.00   0.50    2.00    --  -52.43   0.00  90.00   92
  3  \w    -84.00 -49.00   0.50    2.00    --  -52.43   0.00-120.00   70
  4  \w    -50.00 -24.00   0.50    2.00    --  -52.43 -15.00-180.00   52
  5  \w    -94.00 -54.00   0.50    2.00    --  -52.43 -15.00-180.00   80
  6  \w    -71.00 -46.00   0.50    2.00    --  -52.43 125.00-120.00   50
  7  \w     43.00  85.00   0.50    2.00    --   68.73-125.00 -90.00   84
  8  \w     70.00  95.00   0.50    2.00    --   69.88-125.00 -90.00   50
  9  \w     37.00 104.00   0.50    2.00    --   69.88   0.00 -60.00  134
 10  \w     36.00  73.00   0.50    2.00    --   69.88-125.00  30.00   74
 11  \w     36.00  66.00   0.50    2.00    --   69.88-125.00-150.00   60
 12  \w     82.00 107.00   0.50    2.00    --   75.25  76.00 -34.54   50
 13  \w     65.00 109.00   0.50    2.00    --   75.25-141.00 104.65   88
 14  \w     78.00 111.00   0.50    2.00    --   75.25  21.00-145.95   66
 15  \w     82.00 108.00   0.50    2.00    --   75.25   7.00-173.15   52
 16  \w     54.00  80.00   0.50    2.00    --   75.25   7.00-173.15   52
 17  \w     43.00  86.00   0.50    2.00    --   75.25-111.00 158.23   86
 18  \w     90.00 118.00   0.50    2.00    --   75.25  45.00-116.98   56
 19  \w     86.00 111.00   0.50    2.00    --   75.25  12.00  48.67   50
 20  \w     67.00 117.00   0.50    2.00    --   75.25  19.00 110.00  100
 21  \w     51.00  79.00   0.50    2.00    --   75.25  12.00  48.67   56
 22  \w     41.00  81.00   0.50    2.00    --   75.25 -97.00-170.06   80
 23  \w     42.00 106.00   0.50    2.00    --   75.25   2.00 -34.47  128
 24  \w     91.00 116.00   0.50    2.00    --   75.25  50.00 -85.93   50
 25  \w     72.00 107.00   0.50    2.00    --   75.25  20.00-111.02   70
 26  \w     54.00  84.00   0.50    2.00    --   75.25-104.00 166.94   60
 27  \w     66.00  99.00   0.50    2.00    --   75.25  12.00 -53.26   66
 28  \w     48.00 105.00   0.50    2.00    --   75.25-145.00  -1.33  114
 29  \w     82.00 107.00   0.50    2.00    --   75.25  76.00  16.60   50
 30  \w     53.00  79.00   0.50    2.00    --   75.25   8.00  14.13   52
 31  \w     72.00  99.00   0.50    2.00    --   75.25  21.00 -49.69   54
 32  \w     76.00 101.00   0.50    2.00    --   75.25   7.00 136.30   50
 33  \w     44.00  70.00   0.50    2.00    --   75.25   7.00 136.30   52
 34  \w     81.00 108.00   0.50    2.00    --   75.25  21.00 -30.53   54
 35  \w     39.00  79.00   0.50    2.00    --   75.25-103.00  11.49   80
 36  \w     83.00 108.00   0.50    2.00    --   75.25   8.00  14.13   50
 37  \w     86.00 111.00   0.50    2.00    --   75.25  32.00  42.48   50
 38  \w     44.00  70.00   0.50    2.00    --   75.25-103.00-162.14   52
 39  \w     48.00  80.00   0.50    2.00    --   75.25-105.00-148.33   64
 40  \w     82.00 107.00   0.50    2.00    --   75.25  80.00-134.82   50
 41  \w     37.00  62.00   0.50    2.00    --   75.25 -57.00 174.03   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139696000
_diffrn_orient_matrix_UB_12      0.0551616000
_diffrn_orient_matrix_UB_13      -0.0612632000
_diffrn_orient_matrix_UB_21      0.0648345000
_diffrn_orient_matrix_UB_22      0.0152799000
_diffrn_orient_matrix_UB_23      -0.0010417000
_diffrn_orient_matrix_UB_31      0.0018513000
_diffrn_orient_matrix_UB_32      -0.1259885000
_diffrn_orient_matrix_UB_33      -0.0269157000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.640
_diffrn_reflns_theta_min         3.807
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.412
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.53a (Rigaku Oxford Diffraction, 2020)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.591
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         19051
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0611P)^2^+15.5293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17814
_reflns_number_total             19051
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9715\% 
 around [1.00 -0.00 0.00] (reciprocal) or [0.99 -0.00 0.17] (direct)
;
_cod_data_source_file            d2dt02627a2.cif
_cod_data_source_block           alt_l1
_cod_original_cell_volume        6034.52(11)
_cod_database_code               7711388
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H58 Cl3 La1 N6 O22'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7557(6)
 0.2443(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 N9-H9 = N35-H35
 0.88 with sigma of 0.02
 La1-H9A \\sim La1-H9B
 with sigma of 0.02
4.a Free rotating group:
 O9(H9A,H9B)
4.b Rotating group:
 O10(H10A,H10B)
4.c Ternary CH refined with riding coordinates:
 C7(H7), C33(H33)
4.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B)
4.e Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C16(H16), C18(H18), C19(H19), C20(H20),
 C25(H25), C26(H26), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C49(H49), C50(H50)
4.f X=CH2 refined with riding coordinates:
 C6(H6A,H6B), C32(H32A,H32B)
4.g Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C82(H82A,H82B,
 H82C)
;
_shelx_res_checksum              3606
_shelx_hkl_checksum              4066
_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 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.332
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2