Hypersensitive dual-function luminescence switching of a silver-chalcogenolate cluster-based metal-organic framework
Ren-Wu Huang; Yong-Sheng Wei; Xi-Yan Dong; Xiao-Hui Wu; Chen-Xia Du; Shuang-Quan Zang; Thomas C. W. Mak; Nature Chemistry 9 (2017) 689–697; doi:10.1038/nchem.2718

data_1551434
_publ_section_title
;
 Hypersensitive dual-function luminescence switching of a
 silver-chalcogenolate cluster-based metal-organic framework
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              689
_journal_page_last               697
_journal_paper_doi               10.1038/nchem.2718
_journal_volume                  9
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C80 H104 Ag12 F12 N8 O8 S8, 4(C6 H6)'
_chemical_formula_sum            'C104 H128 Ag12 F12 N8 O8 S8'
_chemical_formula_weight         3397.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.29800(10)
_cell_length_b                   17.29800(10)
_cell_length_c                   20.5393(4)
_cell_measurement_reflns_used    13003
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.9270
_cell_measurement_theta_min      3.6420
_cell_volume                     6145.79(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -19.00   23.40   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755  -99.0000    0.0000 53

  2 omega   38.00   77.20   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661 -178.0000   30.0000 49

  3 omega    9.00   46.60   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   57.0000   90.0000 47

  4 omega  -38.00   23.60   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -57.0000   90.0000 77

  5 omega   -1.00   85.40   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   37.0000   30.0000 108

  6 omega   35.00   60.60   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  178.0000  -90.0000 32

  7 omega    2.00   80.40   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   57.0000 -180.0000 98

  8 omega  -47.00   44.20   0.8000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -77.0000 -120.0000 114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31078
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         29.411
_diffrn_reflns_theta_min         3.670
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.836
_exptl_crystal_description       block
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1516 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.022(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0248P)^2^+12.6339P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                3691
_reflns_number_total             4087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2718-s17.cif
_cod_data_source_block           ag12bpy_benzene
_cod_original_cell_volume        6145.79(14)
_cod_database_code               1551434
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C15 = C16-C15 = C16-C16_$1 = C14-C14_$1
 1.39 with sigma of 0.01
 F1B-C8B \\sim C8B-F2B \\sim F1-C8 \\sim F2-C8
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F2B) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8B) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(F2B)=1-FVAR(1)
 Sof(C8B)=Sof(F1B)=0.5*(1-FVAR(2))
 Sof(C8)=Sof(F1)=0.5*FVAR(2)
 Sof(F2)=FVAR(1)
 Fixed Sof: Ag3(0.25) H3A(0.5) H3B(0.5) H3C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
Comments: The trifluoroacetate anion and the lattice benzene 
molecule were found to be disordered in this structure. 
For trifluoroacetate, two parts were assigned for the 
trifluoromethyl group with a refined occupancy ratio of 
approximately 0.62:0.38. A similar C-F distance refinement 
was applied for all C-F bonds with the "SADI 0.01" command, 
and the thermal vibration parameters were also restrained 
with "ISOR 0.01 0.02". The determination of the lattice benzene 
molecule was completed with the difference Fourier map; 
however, the disorder and high symmetry required the 
assigned benzene molecule to be refined with strong restraints, 
such as "DFIX 1.39 0.01" for the C-C bonds and 
"SIMU 0.01 0.02" for the ADPs.
;
_shelx_res_checksum              5715
_shelx_hkl_checksum              92270