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_7245669
_publ_section_title
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 Achieving stable photoluminescence by double thiacalix[4]arene-capping:
 the lanthanide-oxo cluster core matters
;
_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
'C49 H65 Cl Eu2 N3 O7.5 S4, C45 H56 Cl Eu2 N O8.5 S4, 2(C H4 O), 0.33[CH3OH]'
_chemical_formula_sum            'C96 H129 Cl2 Eu4 N4 O18 S8'
_chemical_formula_weight         2562.24
_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             2022-05-06
_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                69.3320(10)
_cell_angle_beta                 83.0420(10)
_cell_angle_gamma                86.5600(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2472(3)
_cell_length_b                   20.8833(5)
_cell_length_c                   22.7770(5)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      27.497
_cell_measurement_theta_min      2.635
_cell_volume                     5409.5(2)
_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      200.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            114643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         1.926
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8538.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2582
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1228
_refine_ls_number_reflns         24852
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+14.0948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21857
_reflns_number_total             24852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04942b2.cif
_cod_data_source_block           aaaaa
_cod_database_code               7245669
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.724
_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
 O14-H14
 0.87 with sigma of 0.01
 C49-H14
 1.905392 with sigma of 0.02
 Eu3-H14
 2.930138 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Riding coordinates:
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C18(H18), C24(H24), C36(H36), C38(H38), C40(H40), C44(H44),
 C46(H46), C48(H48), C56(H56), C68(H68), C70(H70), C76(H76), C84(H84), C86(H86),
  C92(H92), C96(H96), C51(H51), C53(H53), C31(H31), C33(H33)
4.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
4.d Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C49(H49A,H49B,H49C), C27(H27A,H27B,H27C), C57(H57A,H57B,
 H57C), C15(H15A,H15B,H15C), C2(H2A,H2B,H2C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C17(H17A,H17B,H17C), C69(H69A,H69B,H69C), C35(H35A,H35B,H35C),
 C9(H9A,H9B,H9C), C73(H73A,H73B,H73C), C37(H37A,H37B,H37C), C75(H75A,H75B,H75C),
  C19(H19A,H19B,H19C), C77(H77A,H77B,H77C), C39(H39A,H39B,H39C), C79(H79A,H79B,
 H79C), C5(H5A,H5B,H5C), C81(H81A,H81B,H81C), C41(H41A,H41B,H41C), C83(H83A,
 H83B,H83C), C21(H21A,H21B,H21C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C),
 C11(H11A,H11B,H11C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C23(H23A,H23B,
 H23C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C)
4.e Idealised tetrahedral OH refined as rotating group:
 O17(H17)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 16 electrons were 
found in a volume of 315\%A^3^ in 6 voids per unit cell. 
This is consistent with the presence of 
0.33[CH3OH] per Asymmetric Unit 
which account for 12 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28515
_shelx_fab_checksum              45272
_olex2_submission_special_instructions 'No special instructions were received'