Toroidal moment and dynamical control in luminescent 1D and 3D terbium calixarene compounds
Wang, Hao; Zhu, Zhenhua; La Droitte, Léo; Liao, Wuping; Cador, Olivier; Le Guennic, Boris; Tang, Jinkui; Chemical Science 14 (2023) 7208–7214; doi:10.1039/D3SC00541K

data_1569449
_publ_section_title
;
 Toroidal moment and dynamical control in luminescent 1D and 3D terbium
 calixarene compounds
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              7208
_journal_page_last               7214
_journal_paper_doi               10.1039/D3SC00541K
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C114 H120 O23 S8 Tb4, C H4 O'
_chemical_formula_sum            'C115 H124 O24 S8 Tb4'
_chemical_formula_weight         2782.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-13 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7641(4)
_cell_length_b                   57.5684(16)
_cell_length_c                   36.0789(11)
_cell_measurement_reflns_used    9006
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      54.996
_cell_measurement_theta_min      2.458
_cell_volume                     26418.7(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            58631
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        55.084
_diffrn_reflns_theta_max         55.084
_diffrn_reflns_theta_min         1.966
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    12.000
_exptl_absorpt_correction_T_max  0.301
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             11152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.094
_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     1404
_refine_ls_number_reflns         16159
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+237.3101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12690
_reflns_number_total             16159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00541k2.cif
_cod_data_source_block           lixl
_cod_database_code               1569449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.380
_shelx_estimated_absorpt_t_min   0.266
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O26-C042
 1.4 with sigma of 0.02
 O15-H15
 0.87 with sigma of 0.01
 O6-H6
 0.87 with sigma of 0.01
 O16-H16
 0.87 with sigma of 0.01
 O9-H9
 0.87 with sigma of 0.01
 Tb2-H9
 2.921867 with sigma of 0.02
 C03W-H16
 1.878351 with sigma of 0.02
 Tb4-H15
 2.940298 with sigma of 0.02
 Tb4-H16
 2.867778 with sigma of 0.02
 C5-H9
 1.923761 with sigma of 0.02
 C02U-H6
 1.918698 with sigma of 0.02
 Tb1-H6
 2.896786 with sigma of 0.02
 C02R-H15
 1.877469 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C023 \\sim C02Y \\sim C048 \\sim C04A \\sim C13: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3.8A
O26 \\sim C042: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
O9 \\sim C5: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
4.a Riding coordinates:
 C5(H5A,H5B,H5C)
4.b Aromatic/amide H refined with riding coordinates:
 C01A(H01A), C01C(H01C), C01K(H01K), C01L(H01L), C01M(H01M), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01U(H01U), C01V(H01V), C01Y(H01Y),
 C027(H027), C028(H028), C02B(H02B), C02C(H02C), C02F(H02F), C02Q(H02Q),
 C02T(H02T), C02V(H02V), C032(H032), C033(H033), C034(H034), C038(H038),
 C03C(H03V), C03D(H03W), C03F(H03X), C03G(H03Y), C03J(H03), C03Q(H4), C03R(H5),
 C043(H043)
4.c Idealised Me refined as rotating group:
 C02J(H02A,H02D,H02E), C02R(H02G,H02H,H02I), C02U(H02J,H02K,H02L), C02X(H02M,
 H02N,H02O), C02Z(H02P,H02R,H02S), C031(H03A,H03B,H03C), C035(H03D,H03E,H03F),
 C036(H03G,H03H,H03I), C037(H03J,H03K,H03L), C039(H03M,H03N,H03O), C03A(H03P,
 H03Q,H03R), C03B(H03S,H03T,H03U), C03H(H03Z,H,HA), C03L(H1,HB,HC), C03N(H2,HD,
 HE), C03P(H3,HF,HG), C03U(H7,HH,HI), C03V(H8,HJ,HK), C03W(H10,HL,HM), C03Y(H11,
 HN,HO), C03Z(H12,HP,HQ), C041(H04A,H04B,H04C), C042(H04M,H04N,H04O), C046(H04D,
 H04E,H04F), C1(H1A,H1B,H1C), C048(H04G,H04H,H04I), C04A(H04J,H04K,H04L),
 C13(H13A,H13B,H13C)
4.d Idealised tetrahedral OH refined as rotating group:
 O26(H26)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1248 electrons were 
found in a volume of 5788\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
13[H2O], 2.25[H2O] per Asymmetric Unit 
which account for 1220 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6608
_shelx_fab_checksum              21614
_olex2_submission_special_instructions 'No special instructions were received'