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_1569797
_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 Gd N6 O12 S6, 2[ClO4-], 15[H2O]'
_chemical_formula_sum            'C30 H90 Ag5 Cl2 Gd N6 O35 S6'
_chemical_formula_weight         2054.93
_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                   20.2194(5)
_cell_length_b                   20.2194(5)
_cell_length_c                   20.2194(5)
_cell_measurement_reflns_used    300
_cell_measurement_temperature    120
_cell_measurement_theta_max      43.24
_cell_measurement_theta_min      7.59
_cell_volume                     8266.2(4)
_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      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
 305 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  0.0428
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12902
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.690
_diffrn_reflns_theta_min         4.891
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.069
_exptl_absorpt_correction_T_max  0.1572
_exptl_absorpt_correction_T_min  0.0336
_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    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4084
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 1087 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1083P)^2^+22.2489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.2102
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                3520
_reflns_number_total             4951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03302c2.cif
_cod_data_source_block           L-GdAg5
_cod_depositor_comments
'Adding full bibliography for 1569795--1569800.cif.'
_cod_original_cell_volume        8266.2(6)
_cod_database_code               1569797
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.171
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53169
 0.46831
2. Restrained distances
 S1-C2 = S2-C1
 1.85 with sigma of 0.01
 C7-C2 = C5-C2 = C4-C1 = C9-C1
 1.52 with sigma of 0.0001
 C8-C2 = C3-C1
 1.51 with sigma of 0.0001
 N1-C3
 1.48 with sigma of 0.01
 C8-C6 = C3-C10
 1.46 with sigma of 0.0001
 C7-C5
 2.45 with sigma of 0.01
 C9-C4
 2.45 with sigma of 0.01
 O2-C6 \\sim O1-C6 \\sim O4-C10 \\sim O3-C10
 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: Gd1(0.166667) Gd2(0.166667)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C8(H8)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              25441
_shelx_fab_checksum              94921
_platon_squeeze_special_details
;
A solvent mask was calculated and 1218 electrons were 
found in a volume of 4177\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[ClO4-], 15[H2O] per Formula Unit 
which account for 1000 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'