Achieving stable photoluminescence by double thiacalix[4]arene-capping: the lanthanide-oxo cluster core matters
Lu, Zixiu; Wang, Shujian; Zhuo, Zhu; Li, Guo-Ling; Zhu, Haomiao; Wang, Wei; Huang, You-Gui; Hong, Maochun; RSC Advances 12 (2022) 29151–29161; doi:10.1039/D2RA04942B

data_7245672
_publ_section_title
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 Achieving stable photoluminescence by double thiacalix[4]arene-capping:
 the lanthanide-oxo cluster core matters
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_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              29151
_journal_page_last               29161
_journal_paper_doi               10.1039/D2RA04942B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C80 H136 Gd9 O42 S8, 0.5(C4 H16 O4), 8[Cl]'
_chemical_formula_sum            'C82 H144 Gd9 O44 S8'
_chemical_formula_weight         3505.69
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-07-11 deposited with the CCDC.	2022-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3613(4)
_cell_length_b                   13.3613(4)
_cell_length_c                   46.1864(17)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.33
_cell_volume                     8245.4(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            325276
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         2.018
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.721
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1236 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.8759.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.771
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         4793
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0654P)^2^+38.1236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             4793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04942b2.cif
_cod_data_source_block           bbb
_cod_original_cell_volume        8245.4(6)
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               7245672
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.628
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Gd2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H11A(0.25) H11B(0.25) H11C(0.25) H7(0.25)
4.a Riding coordinates:
 C11(H11A,H11B,H11C), C1(H1C,H1D,H1E), O7(H7)
4.b Rotating group:
 O2(H2A,H2B), O3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6)
4.d X=CH2 refined with riding coordinates:
 O1(H1A,H1B)
4.e Idealised Me refined as rotating group:
 C3(H3C,H3D,H3E), C2(H2C,H2D,H2E)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 268 electrons were 
found in a volume of 2872\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.36[C3H7NO] per Asymmetric Unit 
which account for 269 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41627
_shelx_fab_checksum              52449
_olex2_submission_special_instructions 'No special instructions were received'