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_1569450
_publ_section_title
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 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         '2(C59 H63 N O11.5 S4 Tb2), C3 H7 N O'
_chemical_formula_sum            'C121 H133 N3 O24 S8 Tb4'
_chemical_formula_weight         2905.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                90.609(2)
_cell_angle_beta                 111.829(2)
_cell_angle_gamma                90.189(2)
_cell_formula_units_Z            2
_cell_length_a                   19.1485(7)
_cell_length_b                   19.6598(6)
_cell_length_c                   21.4502(7)
_cell_measurement_reflns_used    9684
_cell_measurement_temperature    179.0
_cell_measurement_theta_max      54.776
_cell_measurement_theta_min      2.248
_cell_volume                     7495.4(4)
_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      179.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            145719
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        55.090
_diffrn_reflns_theta_max         55.090
_diffrn_reflns_theta_min         2.219
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.602
_exptl_absorpt_correction_T_max  0.346
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1481
_refine_ls_number_reflns         18629
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+51.8190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13587
_reflns_number_total             18629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00541k2.cif
_cod_data_source_block           lixl_CCDC1
_cod_database_code               1569450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.417
_shelx_estimated_absorpt_t_min   0.318
_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
 C115-O25
 1.22 with sigma of 0.02
 C115-N1
 1.36 with sigma of 0.02
 N1-C117
 1.46 with sigma of 0.02
 N1-C29
 1.45 with sigma of 0.02
 C119-C111
 1.53 with sigma of 0.02
 C111-C59
 1.53 with sigma of 0.02
 C111-C15
 1.53 with sigma of 0.02
 O7-H7
 0.87 with sigma of 0.01
 O15-H15
 0.87 with sigma of 0.01
 C115-C29
 2.46 with sigma of 0.04
 C115-C117
 2.45 with sigma of 0.04
 C47-H15
 1.918902 with sigma of 0.02
 Tb4-H15
 2.909672 with sigma of 0.02
 C41-H7
 1.915512 with sigma of 0.02
 Tb2-H7
 2.935463 with sigma of 0.02
 N1-C29 \\sim N1-C117
 with sigma of 0.02
 C111-C119 \\sim C111-C15 \\sim C111-C59
 with sigma of 0.02
 C119-C15 \\sim C119-C59 \\sim C15-C59
 with sigma of 0.02
3. Restrained planarity
 C115, O25, N1, C29, C117
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8 \\sim C63 \\sim C21 \\sim C99 \\sim C89 \\sim C2 \\sim C111: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C5 \\sim C97 \\sim C55 \\sim C57 \\sim C107: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
C61 \\sim C83 \\sim C13 \\sim C45 \\sim C53: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
C42 \\sim C82 \\sim C81 \\sim C11 \\sim C39 \\sim C27 \\sim C105 \\sim C113
\\sim C109: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
C1 \\sim C64 \\sim C75 \\sim C5 \\sim C9 \\sim C94 \\sim C97 \\sim C55 \\sim
C57 \\sim C107: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C115 \\sim O25 \\sim N1 \\sim C29 \\sim C117: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C99 \\sim C111 \\sim C59 \\sim C15 \\sim C119: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3.8A
5. Rigid body (RIGU) restrains
 C115, O25, N1, C29, C117
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6.a Riding coordinates:
 C15(H3A,H3B,H3C)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H015), C24(H01D), C26(H01E), C30(H01G), C34(H01J), C36(H01K), C40(H01M),
 C54(H01T), C56(H01U), C62(H01X), C66(H01Z), C72(H022), C80(H026), C88(H02A),
 C90(H02B), C92(H02C), C96(H02E), C102(H02H), C104(H02I), C110(H02L),
 C116(H02O), C120(H02Q), C121(H02R), C31(H02T), C65(H02W), C33(H02X), C67(H02Y),
  C69(H030), C9(H033), C75(H036), C39(H039), C81(H3), C21(H4), C89(H6),
 C115(H5A)
6.c Idealised Me refined as rotating group:
 C71(H03,H,HA), C73(H03A,H03B,H03C), C19(H1,HB,HC), C77(H03D,H03E,H03F),
 C79(H2,HD,HE), C41(H03G,H03H,H03I), C87(H5,HF,HG), C45(H03J,H03K,H03L),
 C91(H03M,H03N,H03O), C23(H03P,H03Q,H03R), C93(H03S,H03T,H03U), C47(H8,HH,HI),
 C95(H9,HJ,HK), C3(H03V,H03W,H03X), C49(H03Y,HL,HM), C25(H10,HN,HO), C101(H11,
 HP,HQ), C51(H03Z,HR,HS), C13(H04A,H04B,H04C), C105(H04M,H04N,H04O), C53(H04D,
 H04E,H04F), C107(H04G,H04H,H04I), C109(H04P,H04Q,H04R), C55(H04J,H04K,H04L),
 C7(H04S,H04T,H04U), C113(H9A,H9B,H9C), C57(H29A,H29B,H29C), C29(H7A,H7B,H7C),
 C117(H6A,H6B,H6C), C59(H4A,H4B,H4C), C119(H2A,H2B,H2C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 387 electrons were 
found in a volume of 2515\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[C3H7NO] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34755
_shelx_fab_checksum              12819
_olex2_submission_special_instructions 'No special instructions were received'