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_1569800
_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-], 12[H2O]'
_chemical_formula_sum            'C30 H84 Ag5 Cl2 Gd N6 O32 S6'
_chemical_formula_weight         2000.89
_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                   20.354(5)
_cell_length_b                   20.354(5)
_cell_length_c                   20.354(5)
_cell_measurement_reflns_used    7014
_cell_measurement_temperature    120
_cell_measurement_theta_max      68.31
_cell_measurement_theta_min      3.76
_cell_volume                     8432(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.86, Darmstadt 2018
;
_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 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      '236 frames, detector distance = 50 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  0.0846
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10054
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.853
_diffrn_reflns_theta_min         3.761
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    16.689
_exptl_absorpt_correction_T_max  0.3227
_exptl_absorpt_correction_T_min  0.0788
_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    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3964
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.799
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.006(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1189P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                2705
_reflns_number_total             4855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03302c2.cif
_cod_data_source_block           D-GdAg5
_cod_depositor_comments
'Adding full bibliography for 1569795--1569800.cif.'
_cod_original_cell_volume        8432(6)
_cod_database_code               1569800
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.388
_shelx_estimated_absorpt_t_min   0.220
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99602
 0.00398
2. Restrained distances
 C9-C10 = C9-C3 = C5-C4 = C5-C2
 1.522 with sigma of 0.0001
 C8-C5 = C9-C6
 1.51 with sigma of 0.0001
 C7-C6 = C8-C1
 1.49 with sigma of 0.0001
 O4-C7 = O3-C7 = O1-C1 = O2-C1
 1.28 with sigma of 0.01
 H10C-H2D
 2.05 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), N2(H2D,
 H2E,H2F), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              22655
_shelx_fab_checksum              27702
_platon_squeeze_special_details
;
A solvent mask was calculated and 1656 electrons were 
found in a volume of 4455\%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'