Highly tunable emission properties of solid-state supramolecular compounds based on Eu mixed-lanthanide complexes and cucurbit[6]uril
Rakhmanova, Mariana; Sukhikh, Taisiya; Kovalenko, Ekaterina; CrystEngComm 26 (2024) 3954–3963; doi:10.1039/D4CE00375F

data_7248890
_publ_section_title
;
 Highly tunable emission properties of solid-state supramolecular
 compounds based on Eu mixed-lanthanide complexes and cucurbit[6]uril
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              3954
_journal_page_last               3963
_journal_paper_doi               10.1039/D4CE00375F
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'2(C18 H28 Eu0.5 N13 O14 Tb0.5), 5(N O3), 6(H2 O)'
_chemical_formula_sum            'C36 H68 Eu N31 O49 Tb'
_chemical_formula_weight         2030.09
_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             2024-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-01 deposited with the CCDC.	2024-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                73.8223(13)
_cell_angle_beta                 87.3313(13)
_cell_angle_gamma                87.7248(12)
_cell_formula_units_Z            2
_cell_length_a                   13.4041(2)
_cell_length_b                   14.4617(2)
_cell_length_c                   18.2115(3)
_cell_measurement_reflns_used    16934
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9160
_cell_measurement_theta_min      2.2430
_cell_volume                     3385.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_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    -43.00  31.00   0.50   17.50    --  -10.11  77.00  30.00  148
  2  \w    -10.00  25.00   0.50   17.50    --  -10.11 -99.00 -90.00   70
  3  \w    -33.00  43.00   0.50   17.50    --   10.74 -77.00 150.00  152
  4  \w      2.00  28.00   0.50   17.50    --   10.74  77.00  60.00   52
  5  \w    -13.00  85.00   0.50   17.50    --   10.74  38.00 -30.00  196
  6  \w    -27.00   2.00   0.50   17.50    --   10.74  19.00 -30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0052050000
_diffrn_orient_matrix_UB_12      -0.0431162000
_diffrn_orient_matrix_UB_13      -0.0113281000
_diffrn_orient_matrix_UB_21      -0.0342295000
_diffrn_orient_matrix_UB_22      0.0189042000
_diffrn_orient_matrix_UB_23      -0.0293902000
_diffrn_orient_matrix_UB_31      0.0401207000
_diffrn_orient_matrix_UB_32      0.0198420000
_diffrn_orient_matrix_UB_33      -0.0255879000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32288
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.100
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       prism
_exptl_crystal_F_000             2042
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         15136
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+3.5158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13176
_reflns_number_total             15136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00375f2.cif
_cod_data_source_block           km780-4
_cod_depositor_comments
'Adding full bibliography for 7248890--7248896.cif.'
_cod_database_code               7248890
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         TbEuC36H36N24O12(H2O)10(NO3)6
_cell_oxdiff_angle_alpha         73.8223(13)
_cell_oxdiff_angle_beta          87.3313(13)
_cell_oxdiff_angle_gamma         87.7248(12)
_cell_oxdiff_length_a            13.4041(2)
_cell_oxdiff_length_b            14.4617(2)
_cell_oxdiff_length_c            18.2115(3)
_cell_oxdiff_measurement_reflns_used 16934
_cell_oxdiff_volume              3385.45(9)
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.667
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Eu2, Tb2}
{Eu1, Tb1}
3. Restrained distances
 H3WB-O61_$1
 2.1 with sigma of 0.04
 N7-O71N \\sim N7-O72N \\sim N7-O73N \\sim N7A-O71A \\sim N7A-O72A \\sim
N7A-O73A \\sim N8-O81N \\sim N8-
 O82N \\sim N8-O83N \\sim N8A-O81A \\sim N8A-O82A \\sim N8A-O83A
 with sigma of 0.01
 O71N-O72N \\sim O72N-O73N \\sim O73N-O71N \\sim O81N-O82N \\sim O82N-O83N
\\sim O83N-O81N
 with sigma of 0.01
4. Restrained planarity
 N7A, O71A, O72A, O73A
 with sigma of 0.03
5. Uiso/Uaniso restraints and constraints
N7 \\sim O71N \\sim O72N \\sim O73N \\sim N7A \\sim O71A \\sim O72A \\sim O73A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
N8 \\sim O81N \\sim O82N \\sim O83N \\sim N8A \\sim O81A \\sim O82A \\sim O83A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
N4 \\sim O41N \\sim O42N \\sim O43N: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
Uanis(Eu2) = Uanis(Tb2)
Uanis(Eu1) = Uanis(Tb1)
6. Others
 Fixed Sof: Eu1(0.5) Eu2(0.5) N7(0.25) O71N(0.25) O72N(0.25) O73N(0.25)
 N7A(0.25) O71A(0.25) O72A(0.25) O73A(0.25) N8(0.25) O81N(0.25) O82N(0.25)
 O83N(0.25) N8A(0.25) O81A(0.25) O82A(0.25) O83A(0.25) Tb2(0.5) Tb1(0.5)
7.a Free rotating group:
 O11M(H11A,H11B), O13M(H13A,H13B), O14M(H14A,H14B), O21M(H21A,H21B), O25M(H25C,
 H25D), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB),
 O5W(H5WA,H5WB), O6W(H6WA,H6WB)
7.b Rotating group:
 O12M(H12A,H12B), O15M(H15A,H15B), O22M(H22A,H22B), O23M(H23A,H23B), O24M(H24A,
 H24B)
7.c Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C23(H23), C24(H24), C33(H33), C34(H34), C43(H43),
 C44(H44), C53(H53), C54(H54), C63(H63), C64(H64)
7.d Secondary CH2 refined with riding coordinates:
 C15(H15C,H15D), C16(H16A,H16B), C25(H25A,H25B), C26(H26A,H26B), C35(H35A,
 H35B), C36(H36A,H36B), C45(H45A,H45B), C46(H46A,H46B), C55(H55A,H55B),
 C56(H56A,H56B), C65(H65A,H65B), C66(H66A,H66B)
;
_shelx_res_checksum              89701
_shelx_hkl_checksum              7120
_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 1.079
_oxdiff_exptl_absorpt_empirical_full_min 0.958