Chiral lanthanide-silver(I) cluster-based metal-organic frameworks exhibiting solvent stability, and tunable photoluminescence.
He, Sheng-Rong; Xu, Han; Chen, Cheng; Wang, Xue-Tao; Lu, Tian-Qi; Cao, Lingyun; Zheng, Jun; Zheng, Xiu-Ying; Nanoscale 15 (2023) 15730–15738; doi:10.1039/d3nr03302c

data_1569795
_publ_section_title
;
 Chiral lanthanide-silver(I) cluster-based metal-organic frameworks
 exhibiting solvent stability, and tunable photoluminescence.
;
_journal_issue                   38
_journal_name_full               Nanoscale
_journal_page_first              15730
_journal_page_last               15738
_journal_paper_doi               10.1039/d3nr03302c
_journal_volume                  15
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H60 Ag5 N6 O12 S6 Tb1, 2[ClO4-], 12[H2O]'
_chemical_formula_sum            'C30 H84 Ag5 Cl2 N6 O32 S6 Tb'
_chemical_formula_weight         2002.56
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.285(3)
_cell_length_b                   20.285(3)
_cell_length_c                   20.285(3)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    150
_cell_measurement_theta_max      69.20
_cell_measurement_theta_min      3.08
_cell_volume                     8347(2)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 206 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            9132
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.929
_diffrn_reflns_theta_max         66.929
_diffrn_reflns_theta_min         4.359
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    15.888
_exptl_absorpt_correction_T_max  0.0716
_exptl_absorpt_correction_T_min  0.0016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.987
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.269
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.1209
_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^)+(0.1831P)^2^+52.6345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2885
_refine_ls_wR_factor_ref         0.3019
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3947
_reflns_number_total             4673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03302c2.cif
_cod_data_source_block           D-TbAg5
_cod_depositor_comments
'Adding full bibliography for 1569795--1569800.cif.'
_cod_original_cell_volume        8346(4)
_cod_database_code               1569795
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.299
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48106
 0.30119 0.16397 0.05378
2. Restrained distances
 N2-C8 = N1-C6
 1.48 with sigma of 0.01
 C5-C1 = C3-C1 = C9-C2 = C9-C7
 1.52 with sigma of 0.0001
 O4-C10 = O3-C10 = O1-C4 = O2-C4
 1.28 with sigma of 0.01
 C9-C8 = C6-C1
 1.51 with sigma of 0.0001
 S2-C9 = S1-C1
 1.85 with sigma of 0.01
 C2-N2
 2.98 with sigma of 0.01
 C3-N1
 2.98 with sigma of 0.01
3. Rigid bond restraints
 C2, C7, C8, N2, C9, O3, C10, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, C4, C6, N1, C1, C3, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C7 \\sim C8 \\sim N2 \\sim C9 \\sim O3 \\sim C10 \\sim O4: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O1 \\sim O2 \\sim C4 \\sim C6 \\sim N1 \\sim C1 \\sim C3 \\sim C5: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C9 \\sim C2 \\sim C7 \\sim C8 \\sim N2 \\sim C10 \\sim S2 \\sim O3 \\sim O4:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(Tb2)=0.33333*(1-FVAR(2))
 Sof(Tb1)=0.33333*FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8)
6.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), N2(H2D,H2E,H2F)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              37291
_shelx_fab_checksum              49824
_platon_squeeze_special_details
;
A solvent mask was calculated and 2552 electrons were 
found in a volume of 4552\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[ClO4-], 12[H2O] per Formula Unit 
which account for 880 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'