A 12-Connected [Y<sub>4</sub>((<i>μ</i><sub>3</sub>-OH)<sub>4</sub>]<sup>8+</sup> Cluster-Based Luminescent Metal-Organic Framework for Selective Turn-on Detection of F<sup>-</sup> in H<sub>2</sub>O.
Li, Juan; Wang, Airong; Qiu, Shiming; Wang, Xiaoli; Li, Jiaming; Molecules (Basel, Switzerland) 28 (2023) 1893–; doi:10.3390/molecules28041893

data_1568610
_publ_section_title
;
 A 12-Connected
 [Y<sub>4</sub>((<i>&#x3bc;</i><sub>3</sub>-OH)<sub>4</sub>]<sup>8+</sup>
 Cluster-Based Luminescent Metal-Organic Framework for Selective Turn-on
 Detection of F<sup>-</sup> in H<sub>2</sub>O.
;
_journal_issue                   4
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              1893
_journal_paper_doi               10.3390/molecules28041893
_journal_volume                  28
_journal_year                    2023
_chemical_formula_moiety         'C112 H70 N8 O59 Y8'
_chemical_formula_sum            'C112 H70 N8 O59 Y8'
_chemical_formula_weight         3183.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   33.7993(10)
_cell_length_b                   33.7993(10)
_cell_length_c                   7.9398(5)
_cell_measurement_reflns_used    7950
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      24.6780
_cell_measurement_theta_min      2.4540
_cell_volume                     9070.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      2.00  46.00   1.00   18.00    --   30.00  54.00-180.00   44
  2  \w    -74.00 109.00   1.00   18.00    --   30.00  54.00 -90.00  183
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202156000
_diffrn_orient_matrix_UB_12      -0.0052422000
_diffrn_orient_matrix_UB_13      -0.0083443000
_diffrn_orient_matrix_UB_21      -0.0027948000
_diffrn_orient_matrix_UB_22      0.0030621000
_diffrn_orient_matrix_UB_23      0.0877180000
_diffrn_orient_matrix_UB_31      -0.0048638000
_diffrn_orient_matrix_UB_32      0.0200741000
_diffrn_orient_matrix_UB_33      -0.0153511000
_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  0.1128
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            33572
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.594
_refine_diff_density_min         -4.683
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         8216
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.1209
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1949P)^2^+83.2242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3069
_refine_ls_wR_factor_ref         0.3291
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                6343
_reflns_number_total             8216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           190610c_sq
_cod_original_cell_volume        9070.4(8)
_cod_database_code               1568610
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.563
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 O9-N2
 1.23 with sigma of 0.02
 N2-O10
 1.23 with sigma of 0.02
 C4-C3
 1.4 with sigma of 0.02
 N1-O3
 1.2 with sigma of 0.02
 C21-C16
 1.4 with sigma of 0.02
 N1-O4
 1.2 with sigma of 0.02
 O12-C28
 1.2 with sigma of 0.02
 C2-C7
 1.4 with sigma of 0.02
 C28-O11
 1.2 with sigma of 0.02
 C12-C11
 1.4 with sigma of 0.02
 O8-C15
 1.2 with sigma of 0.02
 C19-C20
 1.4 with sigma of 0.02
 C15-O7
 1.2 with sigma of 0.02
 C17-C18
 1.4 with sigma of 0.02
 O2-C1
 1.2 with sigma of 0.02
 C6-C5
 1.4 with sigma of 0.02
 C1-O1
 1.2 with sigma of 0.02
 C8-C13
 1.4 with sigma of 0.02
 C10-C9
 1.4 with sigma of 0.02
 C25-C28
 1.53 with sigma of 0.02
 C20-C21
 1.4 with sigma of 0.02
 C2-C1
 1.53 with sigma of 0.02
 C16-C17
 1.4 with sigma of 0.02
 C16-C15
 1.53 with sigma of 0.02
 C18-C19
 1.4 with sigma of 0.02
 C14-C11
 1.53 with sigma of 0.02
 C7-C6
 1.4 with sigma of 0.02
 C25-C26
 1.4 with sigma of 0.02
 C5-C4
 1.4 with sigma of 0.02
 C26-C27
 1.4 with sigma of 0.02
 C3-C2
 1.4 with sigma of 0.02
 C27-C22
 1.4 with sigma of 0.02
 C13-C12
 1.4 with sigma of 0.02
 C22-C23
 1.4 with sigma of 0.02
 C11-C10
 1.4 with sigma of 0.02
 C23-C24
 1.4 with sigma of 0.02
 C9-C8
 1.4 with sigma of 0.02
 C24-C25
 1.4 with sigma of 0.02
 C19-C22
 1.5 with sigma of 0.02
 C8-C5
 1.5 with sigma of 0.02
 C17-N2
 1.47 with sigma of 0.02
 N1-C3
 1.47 with sigma of 0.02
4. Restrained planarity
 C25, C26, C27, C22, C23, C24
 with sigma of 0.1
 C2, C7, C6, C5, C4, C3
 with sigma of 0.1
 C19, C20, C21, C16, C17, C18
 with sigma of 0.1
 C8, C13, C12, C11, C10, C9
 with sigma of 0.1
5. 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
6. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(O12) = Uanis(O8) = Uanis(O7) = Uanis(O9) = Uanis(O10) =
Uanis(O3) = Uanis(O4) = Uanis(O1) = Uanis(O2) = Uanis(O13) = Uanis(O6) =
Uanis(O5) = Uanis(O16) = Uanis(O17) = Uanis(O14) = Uanis(O15) = Uanis(N1) =
Uanis(N2)
Uanis(C28) = Uanis(C15) = Uanis(C14) = Uanis(C1)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C22) = Uanis(C23) = Uanis(C24) =
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C16) = Uanis(C17) = Uanis(C18) =
Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) =
Uanis(C8) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9)
7. Others
 Fixed Sof: O16(0.5) H16A(0.5) H16B(0.5) H17A(0.25) H17B(0.25)
8.a Riding coordinates:
 O16(H16A,H16B), O14(H14), O17(H17A,H17B), O13(H13A), O15(H15)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C6(H6), C12(H12), C20(H20), C10(H10), C26(H26), C18(H18),
 C4(H4), C27(H27), C13(H13), C9(H9), C24(H24), C23(H23)
;
_shelx_res_checksum              26987
_shelx_hkl_checksum              47998
_shelx_fab_checksum              57437
_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 2.155
_oxdiff_exptl_absorpt_empirical_full_min 0.562