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_1551442
_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_formula_moiety         'C80 H104 Ag12 F12 N8 O8 S8, 2(C8 H10)'
_chemical_formula_sum            'C96 H124 Ag12 F12 N8 O8 S8'
_chemical_formula_weight         3296.94
_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   mixed
_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                   17.26030(10)
_cell_length_b                   17.26030(10)
_cell_length_c                   20.5849(5)
_cell_measurement_reflns_used    17946
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6420
_cell_measurement_theta_min      2.8230
_cell_volume                     6132.61(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.937
_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    -14.00  36.00   0.50    3.50    --    7.30 -77.00 -30.00  100
  2  \w    -33.00  24.00   0.50    3.50    --   -7.10 -82.00  90.00  114
  3  \w    -33.00  33.00   0.50    3.50    --    7.30 -82.00-120.00  132
  4  \w    -44.00  36.00   0.50    3.50    --    7.30 -77.00 120.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro:Kappa single'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092730000
_diffrn_orient_matrix_UB_12      0.0059574000
_diffrn_orient_matrix_UB_13      0.0331932000
_diffrn_orient_matrix_UB_21      0.0117713000
_diffrn_orient_matrix_UB_22      0.0392171000
_diffrn_orient_matrix_UB_23      -0.0026580000
_diffrn_orient_matrix_UB_31      -0.0382823000
_diffrn_orient_matrix_UB_32      0.0106577000
_diffrn_orient_matrix_UB_33      -0.0088717000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32617
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         32.827
_diffrn_reflns_theta_min         2.818
_diffrn_source                   MM007HF-DW
_diffrn_source_type              'Microfocus Rotating Anode X-ray Source'
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2129 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.039(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5358
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+6.7097P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                5061
_reflns_number_total             5358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2718-s25.cif
_cod_data_source_block           ag12bpy_p-xylene
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6132.61(17)
_cod_database_code               1551442
_chemical_oxdiff_formula         'C80 H104 O8 N8 S8 Ag12'
_chemical_oxdiff_usercomment     st
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.726
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
 C9-F1 \\sim C9-F2 \\sim C9-F1B \\sim C9-F2B
 with sigma of 0.005
 F1B-F2B \\sim F2-F1 \\sim F2B_$1-F2B \\sim F2B-F1B \\sim F1-F2 \\sim F2-F2_$1
 with sigma of 0.01
 C4-C6 \\sim C4-C7
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(F2B) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
4. Others
 Sof(F2B)=1-FVAR(1)
 Sof(F1B)=0.5*(1-FVAR(2))
 Sof(F1)=0.5*FVAR(2)
 Sof(F2)=FVAR(1)
 Fixed Sof: Ag3(0.25) H3A(0.5) H3B(0.5) H3C(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
 C15(0.25) H15A(0.25) H15B(0.25) H15C(0.25) C16(0.25) C17(0.5) H17(0.5)
 C18(0.5) H18(0.5) C19(0.25) C20(0.25) H20A(0.25) H20B(0.25) H20C(0.25)
 Fixed X: C15(0) C16(0) C19(0) C20(0)
 Fixed Z: C15(1) C16(1) C19(1) C20(1)
5.a Riding coordinates:
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C14(H14), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C)
Comments: Several groups, including the trifluoroacetate anion, 
the t-butyl mercaptan anion and the guest molecule p-xylene, 
were involved in disorder. Various strategies for the disorder 
treatments were applied to different groups. The trifluoroacetate 
was treated with relatively strong geometrical and ADP restraints 
using "SADI 0.005" or "SADI 0.01" and "ISOR 0.01" or 
"ISOR 0.005", respectively. One t-butyl mercaptan anion also 
suffered positional disorder due to the symmetry. "PART -1" was 
used to suppress the symmetry according to the chemistry with 
0.5 occupancy. The separated carbon atoms in each part with bad 
ADPs were not split more, but they were restrained by the hard 
"ISOR 0.003 0.006" command. For the p-xylene group, the atoms 
were clearly determined from the difference Fourier map. However, 
due to the high disorder, the geometrical symmetry of the molecule 
and the lattice symmetry, only a simple model was created to 
present the major part of the molecule, for which very the strong 
restraints "ISOR 0.005 0.01" or "ISOR 0.01 0.02" were used.
;
_shelx_res_checksum              35586
_shelx_hkl_checksum              51575